DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 11:59:21 2019) ID: 3668; threads 40; handles 809; mem 516376.00 (1204708.00)kB; time: 1w 4d 22h 10m 9s MEMORY INFO: Memory PF:73.0, Ph:539.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:504.3,peak PF: 700.2, WS: 472.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:76.0, Ph:541.0, V:1178.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:506.1,peak PF: 700.2, WS: 473.8, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 11:59:21 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000127 0.000100 0.000207 ) 0.065981 0.091690 0.025911 ( 0.000145 0.000115 0.000237 ) 0.044418 0.058869 0.132122 ( 0.000104 0.000082 0.000170 ) 7.34808 ( 0.01055 ) 7.34732 ( 0.01206 ) 7.36303 ( 0.01208 ) 119.94370 ( 0.17533 ) 119.84600 ( 0.16433 ) 90.15964 ( 0.12439 ) V = 281.59 Selected cell (from UM rr/UM ttt/UM f): 44 7.3481 7.3473 7.3630 119.9437 119.8460 90.1596 aP Cross checking gral lattice... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 11:59:22 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000127 0.000100 0.000207 ) 0.065981 0.091690 0.025911 ( 0.000145 0.000115 0.000237 ) 0.044418 0.058869 0.132122 ( 0.000104 0.000082 0.000170 ) M - matrix: 0.013943 0.004665 0.009248 ( 0.000031 0.000020 0.000029 ) 0.004665 0.013973 0.009277 ( 0.000020 0.000025 0.000028 ) 0.009248 0.009277 0.018494 ( 0.000029 0.000028 0.000047 ) unit cell: 7.348(11) 7.347(12) 7.363(12) 119.94(18) 119.85(16) 90.16(12) V = 281.6(7) 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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb PROFFITPEAK info: 99 peaks in the peak location table UB fit with 59 obs out of 65 (total:65,skipped:0) (90.77%) UB - matrix: 0.087150 -0.045842 0.018893 ( 0.000145 0.000176 0.000285 ) 0.065893 0.091516 0.025924 ( 0.000122 0.000148 0.000240 ) 0.044631 0.058487 0.132272 ( 0.000155 0.000188 0.000305 ) M - matrix: 0.013929 0.004645 0.009258 ( 0.000033 0.000026 0.000039 ) 0.004645 0.013897 0.009243 ( 0.000026 0.000039 0.000040 ) 0.009258 0.009243 0.018525 ( 0.000039 0.000040 0.000082 ) unit cell: 7.354(13) 7.361(14) 7.354(18) 119.9(2) 119.9(2) 90.16(15) V = 282(1) UB fit with 59 obs out of 65 (total:65,skipped:0) (90.77%) UB - matrix: 0.087150 -0.045842 0.018893 ( 0.000145 0.000176 0.000285 ) 0.065893 0.091516 0.025924 ( 0.000122 0.000148 0.000240 ) 0.044631 0.058487 0.132272 ( 0.000155 0.000188 0.000305 ) M - matrix: 0.013929 0.004645 0.009258 ( 0.000033 0.000026 0.000039 ) 0.004645 0.013897 0.009243 ( 0.000026 0.000039 0.000040 ) 0.009258 0.009243 0.018525 ( 0.000039 0.000040 0.000082 ) unit cell: 7.354(13) 7.361(14) 7.354(18) 119.9(2) 119.9(2) 90.16(15) V = 282(1) OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 UB - matrix: 0.087139 -0.045907 0.018778 ( 0.000134 0.000163 0.000265 ) 0.065923 0.091468 0.026059 ( 0.000084 0.000103 0.000166 ) 0.044690 0.058398 0.132313 ( 0.000138 0.000168 0.000273 ) M - matrix: 0.013936 0.004639 0.009267 ( 0.000029 0.000022 0.000034 ) 0.004639 0.013884 0.009248 ( 0.000022 0.000031 0.000034 ) 0.009267 0.009248 0.018538 ( 0.000034 0.000034 0.000073 ) UB fit with 59 obs out of 65 (total:65,skipped:0) (90.77%) unit cell: 7.354(12) 7.367(11) 7.356(16) 119.92(19) 119.9(2) 90.10(13) V = 282.2(9) UB fit with 59 obs out of 65 (total:65,skipped:0) (90.77%) UB - matrix: 0.087139 -0.045907 0.018778 ( 0.000134 0.000163 0.000265 ) 0.065923 0.091468 0.026059 ( 0.000084 0.000103 0.000166 ) 0.044690 0.058398 0.132313 ( 0.000138 0.000168 0.000273 ) M - matrix: 0.013936 0.004639 0.009267 ( 0.000029 0.000022 0.000034 ) 0.004639 0.013884 0.009248 ( 0.000022 0.000031 0.000034 ) 0.009267 0.009248 0.018538 ( 0.000034 0.000034 0.000073 ) unit cell: 7.354(12) 7.367(11) 7.356(16) 119.92(19) 119.9(2) 90.10(13) V = 282.2(9) 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 65 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Run 1 Omega scan: (-97.000 - -72.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 466 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 59 obs out of 65 (total:65,skipped:0) (90.77%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb 0 of 48 peaks identified as outliers and rejected 48 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 48 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 48 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 3.14 | 5 | 0.878 ( 0.074) | 0.888 ( 0.087) | 0.699 ( 0.336) | 3.11- 2.12 | 5 | 0.822 ( 0.108) | 0.810 ( 0.178) | 1.175 ( 0.468) | 2.11- 1.58 | 5 | 0.820 ( 0.068) | 0.794 ( 0.159) | 0.680 ( 0.185) | 1.58- 1.36 | 5 | 0.895 ( 0.080) | 0.967 ( 0.126) | 0.797 ( 0.526) | 1.36- 1.19 | 5 | 0.960 ( 0.023) | 1.076 ( 0.048) | 1.002 ( 0.507) | 1.16- 0.92 | 5 | 1.017 ( 0.049) | 1.095 ( 0.073) | 1.315 ( 0.493) | 0.89- 0.88 | 5 | 0.970 ( 0.085) | 1.046 ( 0.098) | 1.117 ( 0.506) | 0.88- 0.73 | 5 | 0.969 ( 0.058) | 1.013 ( 0.145) | 1.234 ( 0.416) | 0.73- 0.72 | 5 | 1.025 ( 0.017) | 0.963 ( 0.110) | 1.367 ( 0.480) | 0.69- 0.68 | 3 | 0.957 ( 0.005) | 0.997 ( 0.116) | 1.386 ( 0.579) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.68 | 48 | 0.930 ( 0.097) | 0.964 ( 0.157) | 1.064 ( 0.523) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 48 obs out of 48 (total:48,skipped:0) (100.00%) UB - matrix: 0.087336 -0.045820 0.019146 ( 0.000082 0.000097 0.000158 ) 0.065828 0.091684 0.026566 ( 0.000069 0.000082 0.000133 ) 0.044274 0.058108 0.132052 ( 0.000088 0.000105 0.000171 ) M - matrix: 0.013921 0.004606 0.009267 ( 0.000019 0.000014 0.000022 ) 0.004606 0.013882 0.009232 ( 0.000014 0.000021 0.000022 ) 0.009267 0.009232 0.018510 ( 0.000022 0.000022 0.000046 ) unit cell: 7.363(7) 7.364(8) 7.369(10) 119.95(13) 120.07(13) 89.90(8) V = 282.7(6) OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 UB - matrix: 0.087306 -0.045776 0.019089 ( 0.000072 0.000086 0.000140 ) 0.065925 0.091844 0.026584 ( 0.000043 0.000051 0.000083 ) 0.044402 0.058282 0.132192 ( 0.000079 0.000094 0.000153 ) M - matrix: 0.013940 0.004646 0.009289 ( 0.000016 0.000012 0.000018 ) 0.004646 0.013928 0.009272 ( 0.000012 0.000016 0.000018 ) 0.009289 0.009272 0.018546 ( 0.000018 0.000018 0.000041 ) UB fit with 48 obs out of 48 (total:48,skipped:0) (100.00%) unit cell: 7.360(6) 7.358(6) 7.365(9) 119.96(10) 120.03(11) 90.01(7) V = 282.1(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - -72.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 463 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 48 obs out of 48 (total:48,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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb 0 of 48 peaks identified as outliers and rejected 48 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 48 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 48 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 3.12 | 5 | 0.878 ( 0.073) | 0.887 ( 0.085) | 0.732 ( 0.302) | 3.12- 2.38 | 5 | 0.802 ( 0.075) | 0.798 ( 0.153) | 1.282 ( 0.786) | 2.11- 1.58 | 5 | 0.847 ( 0.096) | 0.843 ( 0.184) | 0.715 ( 0.193) | 1.58- 1.35 | 5 | 0.874 ( 0.078) | 0.928 ( 0.165) | 0.608 ( 0.230) | 1.35- 1.19 | 5 | 0.968 ( 0.022) | 1.069 ( 0.054) | 1.223 ( 0.517) | 1.19- 1.00 | 5 | 0.993 ( 0.051) | 1.098 ( 0.076) | 1.107 ( 0.534) | 0.92- 0.88 | 5 | 0.962 ( 0.091) | 1.050 ( 0.070) | 1.176 ( 0.579) | 0.88- 0.73 | 5 | 0.969 ( 0.058) | 1.012 ( 0.144) | 1.235 ( 0.415) | 0.73- 0.72 | 5 | 1.026 ( 0.017) | 0.962 ( 0.108) | 1.368 ( 0.478) | 0.69- 0.68 | 3 | 0.957 ( 0.005) | 1.003 ( 0.123) | 1.356 ( 0.597) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.68 | 48 | 0.926 ( 0.096) | 0.963 ( 0.157) | 1.069 ( 0.559) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.0 | 5 | 0.955 ( 0.020) | 1.024 ( 0.045) | 1.240 ( 0.506) | 12.5-14.4 | 5 | 0.968 ( 0.042) | 1.060 ( 0.097) | 0.800 ( 0.149) | 16.4-19.0 | 5 | 0.952 ( 0.067) | 1.069 ( 0.071) | 0.994 ( 0.584) | 20.6-24.7 | 5 | 0.983 ( 0.055) | 1.087 ( 0.098) | 0.845 ( 0.327) | 25.1-27.4 | 5 | 0.963 ( 0.067) | 1.012 ( 0.061) | 1.215 ( 0.542) | 27.5-34.3 | 5 | 0.880 ( 0.077) | 0.932 ( 0.131) | 0.951 ( 0.555) | 36.2-37.1 | 5 | 0.866 ( 0.124) | 0.800 ( 0.119) | 1.641 ( 0.728) | 37.5-39.3 | 5 | 0.913 ( 0.059) | 0.947 ( 0.122) | 1.151 ( 0.575) | 39.3-41.0 | 5 | 0.910 ( 0.133) | 0.868 ( 0.215) | 1.115 ( 0.293) | 41.2-43.3 | 3 | 0.837 ( 0.146) | 0.747 ( 0.105) | 0.513 ( 0.146) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-43.3 | 48 | 0.926 ( 0.096) | 0.963 ( 0.157) | 1.069 ( 0.559) | Fitted profile normalization line parameters e1 dimension: a=-0.0027 b=1.14 e2 dimension: a=-0.0093 b=1.34 e3 dimension: a=0.0055 b=1.02 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 3503 lp-corr: 3313 Maximum peak integral for reflections I/sig<= 100 - raw: 458425 lp-corr: 293035 Maximum peak integral for reflections I/sig<= 10000 - raw: 6303795 lp-corr: 952931 PROFFITPEAK - Finished at Wed Aug 21 11:59:26 2019 PROFFITMAIN - Started at Wed Aug 21 11:59:26 2019 OTKP changes: 48 1 1 1 UB - matrix: 0.087317 -0.045789 0.019057 ( 0.000071 0.000085 0.000140 ) 0.065912 0.091837 0.026552 ( 0.000048 0.000058 0.000095 ) 0.044381 0.058308 0.132256 ( 0.000077 0.000093 0.000154 ) M - matrix: 0.013938 0.004643 0.009284 ( 0.000015 0.000012 0.000019 ) 0.004643 0.013930 0.009277 ( 0.000012 0.000017 0.000019 ) 0.009284 0.009277 0.018560 ( 0.000019 0.000019 0.000041 ) UB fit with 48 obs out of 48 (total:48,skipped:0) (100.00%) unit cell: 7.357(6) 7.358(6) 7.360(9) 119.97(11) 119.99(11) 90.01(7) V = 281.8(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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: (-97.000 - -72.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 458 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.087317 -0.045789 0.019057 ( 0.000071 0.000085 0.000140 ) 0.065912 0.091837 0.026552 ( 0.000048 0.000058 0.000095 ) 0.044381 0.058308 0.132256 ( 0.000077 0.000093 0.000154 ) M - matrix: 0.013938 0.004643 0.009284 ( 0.000015 0.000012 0.000019 ) 0.004643 0.013930 0.009277 ( 0.000012 0.000017 0.000019 ) 0.009284 0.009277 0.018560 ( 0.000019 0.000019 0.000041 ) UB fit with 48 obs out of 48 (total:48,skipped:0) (100.00%) unit cell: 7.357(6) 7.358(6) 7.360(9) 119.97(11) 119.99(11) 90.01(7) V = 281.8(5) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: 0.087317 -0.045789 0.019057 ( 0.000071 0.000085 0.000140 ) 0.065912 0.091837 0.026552 ( 0.000048 0.000058 0.000095 ) 0.044381 0.058308 0.132256 ( 0.000077 0.000093 0.000154 ) M - matrix: 0.013938 0.004643 0.009284 ( 0.000015 0.000012 0.000019 ) 0.004643 0.013930 0.009277 ( 0.000012 0.000017 0.000019 ) 0.009284 0.009277 0.018560 ( 0.000019 0.000019 0.000041 ) UB fit with 48 obs out of 48 (total:48,skipped:0) (100.00%) unit cell: 7.357(6) 7.358(6) 7.360(9) 119.97(11) 119.99(11) 90.01(7) V = 281.8(5) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 12 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof 235 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 11:59:27 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - -72.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-318.0000 max=6134187.0000 PROFFIT INFO: signal sum lp corr: min=-244.5177 max=815648.5383 PROFFIT INFO: background sum: min=375.0000 max=4204.0000 PROFFIT INFO: background sum sig2: min=572.0000 max=4422.0000 PROFFIT INFO: num of signal pixels: min=54 max=402 PROFFIT INFO: Inet: min=-391.2284 max=1305037.7500 PROFFIT INFO: sig(Inet): min=92.1702 max=14978.3867 PROFFIT INFO: Inet/sig(Inet): min=-0.54 max=125.14 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 19 78 125 148 160 184 195 208 222 235 235 Percent 8.1 33.2 53.2 63.0 68.1 78.3 83.0 88.5 94.5 100.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 235 100.00 (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 235 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1305038- 142472 23 382389.71 70.97 100.00 140691- 5287 23 28337.25 19.65 100.00 5027- 2061 23 3036.41 8.37 91.30 2044- 1319 23 1612.53 3.67 60.87 1303- 888 23 1084.62 2.02 0.00 883- 585 23 741.70 1.85 13.04 583- 384 23 493.36 1.47 13.04 378- 127 23 271.60 0.74 0.00 124- 47 23 82.55 0.26 0.00 37- -391 28 -112.14 -0.18 0.00 ------------------------------------------------------------------------------------ 1305038- -391 235 40902.14 10.65 37.02 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 23 140369.84 20.48 78.26 1.64- 1.26 23 26335.10 13.30 65.22 1.26- 1.04 23 77405.43 20.82 65.22 1.04- 0.95 23 13558.70 4.82 21.74 0.95- 0.88 23 51230.79 15.47 47.83 0.88- 0.80 23 33938.39 9.68 30.43 0.80- 0.74 23 8116.74 3.26 13.04 0.74- 0.71 23 49124.91 14.35 30.43 0.71- 0.67 23 17195.30 5.73 21.74 0.67- 0.64 28 524.07 0.71 3.57 ------------------------------------------------------------------------------------ 6.00- 0.64 235 40902.14 10.65 37.02 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 11:59:27 2019 Sorting 235 observations 4 unique observations with > 7.00 F2/sig(F2) 235 observations in 1 runs Run # start # end # total # 1 0 24 25 Total number of frames 25 Maximum number of 4 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 235 observations in 1 runs Run # start # end # total # 1 0 3 4 Total number of frames 4 54 observations > 7.00 F2/sig(F2) 54 observations in 1 runs Run # start # end # total # 1 0 3 4 Total number of frames 4 Removing 'redundancy=1' reflections Average redundancy: 2.0 (Out of 54 removed 46 = 8, unique = 4) Not enough coverage in data - scaling will not be applied ! SCALE3 WARNING: ABSPACK failed due to insufficient data coverage PROFFIT INFO: Inet (after scale3 abspack): min=-391.2284 max=1305037.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=92.1702 max=14978.3867 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 0, Friedel: 1 Min/max for: run:1/1 frame:1/25 235 reflections read from tmp file 227 reflections are rejected (0 as outliers, 227 as groups of 1 refl) Redundancy: 1 2+ Number of groups: 0 4 Initial Chi^2= 0.37004 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.16854 Current error model SIG(F2)^2 = 42.86*I_RAW + 1893.22*I_BACK+(0.13489*)^2 Negative value encountered! Resetting parameters to initial values... Cycle 2, Chi^2= 0.56156 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.07805*)^2 Cycle 3, Chi^2= 0.92888 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.05563*)^2 Cycle 4, Chi^2= 0.81296 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.06120*)^2 Cycle 5, Chi^2= 0.84238 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.05969*)^2 Cycle 6, Chi^2= 0.83444 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.06009*)^2 Cycle 7, Chi^2= 0.83655 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.05998*)^2 Final Chi^2= 0.83655 Final error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.05998*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1305038- 142472 23 382389.71 16.14 100.00 140691- 5287 23 28337.25 12.27 100.00 5027- 2061 23 3036.41 7.74 100.00 2044- 1319 23 1612.53 5.24 100.00 1303- 888 23 1084.62 3.73 95.65 883- 585 23 741.70 3.73 82.61 583- 384 23 493.36 3.25 34.78 378- 127 23 271.60 3.00 30.43 124- 47 23 82.55 1.47 8.70 37- -391 28 -112.14 -0.66 0.00 ------------------------------------------------------------------------------------ 1305038- -391 235 40902.14 5.46 63.83 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 23 140369.84 10.08 91.30 1.64- 1.26 23 26335.10 7.66 78.26 1.26- 1.04 23 77405.43 6.89 82.61 1.04- 0.95 23 13558.70 3.85 47.83 0.95- 0.88 23 51230.79 6.70 86.96 0.88- 0.80 23 33938.39 4.29 56.52 0.80- 0.74 23 8116.74 3.34 47.83 0.74- 0.71 23 49124.91 7.17 69.57 0.71- 0.67 23 17195.30 3.80 56.52 0.67- 0.64 28 524.07 1.61 28.57 ------------------------------------------------------------------------------------ 6.00- 0.64 235 40902.14 5.46 63.83 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 23 140369.84 10.08 91.30 6.00- 1.26 46 83352.47 8.87 84.78 6.00- 1.04 69 81370.12 8.21 84.06 6.00- 0.95 92 64417.27 7.12 75.00 6.00- 0.88 115 61779.97 7.04 77.39 6.00- 0.80 138 57139.71 6.58 73.91 6.00- 0.74 161 50136.43 6.12 70.19 6.00- 0.71 184 50009.99 6.25 70.11 6.00- 0.67 207 46363.91 5.98 68.60 6.00- 0.64 235 40902.14 5.46 63.83 ------------------------------------------------------------------------------------ 6.00- 0.64 235 40902.14 5.46 63.83 Scale applied to data: s=0.766261 (maximum obs:1305037.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.045; Rsigma 0.065: data 235 -> merged 231 With outlier rejection... Rint 0.045; Rsigma 0.065: data 235 -> merged 231 Rejected total: 0, method kkm 0, method Blessing 0 Completeness direct cell (a, b, c) = (7.357, 7.358, 7.360), (alpha, beta, gamma) = (119.973, 119.993, 90.013) wavelength: 0.709300 dmin, dmax value (Ang): 0.637010, 6.008518 completeness table (Laue group: P1, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.39 31 214 1.13 14.49 35 1.39 - 1.14 28 214 1.00 13.08 28 1.14 - 0.97 25 214 1.00 11.68 25 0.97 - 0.88 22 214 1.00 10.28 22 0.88 - 0.81 20 214 1.00 9.35 20 0.81 - 0.78 22 214 1.00 10.28 22 0.78 - 0.73 13 214 1.00 6.07 13 0.73 - 0.70 25 214 1.00 11.68 25 0.70 - 0.67 13 214 1.00 6.07 13 0.67 - 0.65 23 216 1.00 10.65 23 --------------------------------------------------------------- 7.36 - 0.65 222 2142 1.02 10.36 226 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 11:59:27 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.357241 7.357848 7.360111 119.9731 119.9929 90.0132 235 Reflections read from file xs2212a.hkl 234 Reflections used for space-group determination (up to diffraction limit of 0.64A); mean (I/sigma) = 5.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 115 120 117 122 176 157 157 234 N (int>3sigma) = 0 65 71 90 64 113 103 107 150 Mean intensity = 0.0 1.0 1.1 1.6 1.0 1.2 26.8 39.1 31.5 Mean int/sigma = 0.0 3.9 4.0 5.2 3.7 4.4 5.5 5.8 5.5 Lattice type: P chosen Volume: 281.84 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 Unitcell: 7.357 7.358 7.359 60.01 60.02 89.99 Niggli form: a.a = 54.129 b.b = 54.138 c.c = 54.162 b.c = 27.068 a.c = 27.060 a.b = 0.012 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.059 CUBIC F-lattice R(int) = 0.068 [ 87] Vol = 1127.4 Cell: 10.406 10.404 10.413 90.00 90.02 90.00 Volume: 1127.37 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.043 TETRAGONAL I-lattice R(int) = 0.061 [ 15] Vol = 563.7 Cell: 7.360 7.360 10.406 89.99 89.98 89.95 Volume: 563.69 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.016 TETRAGONAL I-lattice R(int) = 0.069 [ 24] Vol = 563.7 Cell: 7.357 7.358 10.413 89.99 89.98 89.99 Volume: 563.69 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.015 ORTHORHOMBIC F-lattice R(int) = 0.070 [ 34] Vol = 1127.4 Cell: 10.406 10.404 10.413 90.00 90.02 90.00 Volume: 1127.37 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.049 ORTHORHOMBIC I-lattice R(int) = 0.075 [ 27] Vol = 563.7 Cell: 10.406 7.360 7.360 89.95 89.98 89.99 Volume: 563.69 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.013 ORTHORHOMBIC I-lattice R(int) = 0.070 [ 42] Vol = 563.7 Cell: 7.357 7.358 10.413 90.01 90.02 89.99 Volume: 563.69 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.011 MONOCLINIC I-lattice R(int) = 0.061 [ 14] Vol = 563.7 Cell: 7.359 10.404 7.362 90.00 90.04 90.01 Volume: 563.69 Matrix:-1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.019 MONOCLINIC I-lattice R(int) = 0.075 [ 11] Vol = 563.7 Cell: 7.360 10.406 7.360 90.02 90.05 89.99 Volume: 563.69 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.013 MONOCLINIC I-lattice R(int) = 0.017 [ 18] Vol = 563.7 Cell: 7.358 7.357 10.413 89.98 90.01 90.01 Volume: 563.69 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.013 MONOCLINIC I-lattice R(int) = 0.068 [ 27] Vol = 563.7 Cell: 7.357 7.358 10.413 89.99 90.02 90.01 Volume: 563.69 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.045 [ 4] Vol = 281.8 Cell: 7.357 7.358 7.359 60.01 60.02 89.99 Volume: 281.84 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 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 0 117 0 160 157 234 N (int>3sigma) = 0 0 0 0 90 0 104 103 150 Mean intensity = 0.0 0.0 0.0 0.0 1.6 0.0 37.6 26.8 31.5 Mean int/sigma = 0.0 0.0 0.0 0.0 5.2 0.0 5.6 5.5 5.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 7.054 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 1 1 19 38 N I>3s 1 1 2 31 0.1 0.1 -0.0 2.5 3.4 3.4 0.5 7.2 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 0.067 83 Fd-3m 1 1 227 C N N N N 37 2284 0.065 128 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.406338 10.403941 10.412918 90.0037 90.0195 90.0047 ZERR 1.00 0.015056 0.002458 0.027268 0.2745 0.0012 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1305038- 138453 25 25 25 1.0 362964.30 16.07 0.000 0.000 119952- 3126 28 28 25 1.1 14295.60 11.28 0.049 0.049 3116- 1695 26 26 25 1.0 2330.36 6.58 0.020 0.020 1565- 1078 25 25 25 1.0 1314.98 4.36 0.000 0.000 1074- 718 25 25 25 1.0 876.90 3.78 0.000 0.000 716- 461 25 25 25 1.0 575.69 3.53 0.000 0.000 458- 173 25 25 25 1.0 332.29 2.98 0.000 0.000 169- 54 25 25 25 1.0 100.91 1.70 0.000 0.000 53- -391 31 31 31 1.0 -96.42 -0.48 0.000 0.000 ------------------------------------------------------------------------------------------- 1305038- -391 235 235 231 1.0 40902.14 5.46 0.045 0.045 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-1.57 29 29 25 1.2 130538.63 10.63 0.045 0.045 0.061 1.46-1.19 25 25 25 1.0 42639.48 6.41 0.000 0.000 0.063 1.16-1.01 25 25 25 1.0 30606.49 4.88 0.000 0.000 0.065 1.01-0.91 25 25 25 1.0 35394.83 5.41 0.000 0.000 0.066 0.91-0.82 25 25 25 1.0 55238.66 6.79 0.000 0.000 0.065 0.82-0.78 25 25 25 1.0 7321.25 2.80 0.000 0.000 0.084 0.78-0.72 25 25 25 1.0 27116.40 5.27 0.000 0.000 0.069 0.72-0.67 25 25 25 1.0 34142.26 5.54 0.000 0.000 0.070 0.67-0.64 31 31 31 1.0 480.62 1.51 0.000 0.000 0.373 ------------------------------------------------------------------------------------------------------ inf-0.64 235 235 231 1.0 40902.14 5.46 0.045 0.045 0.065 inf-0.66 226 226 222 1.0 42525.35 5.65 0.045 0.045 0.065 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-1.57 29 162 25 15.4 1.2 130538.63 12.08 0.045 0.055 1.46-1.19 25 181 25 13.8 1.0 42639.48 6.41 0.000 0.000 1.16-1.01 25 224 25 11.2 1.0 30606.49 4.88 0.000 0.000 1.01-0.91 25 212 25 11.8 1.0 35394.83 5.41 0.000 0.000 0.91-0.82 25 253 25 9.9 1.0 55238.66 6.79 0.000 0.000 0.82-0.78 25 242 25 10.3 1.0 7321.25 2.80 0.000 0.000 0.78-0.72 25 248 25 10.1 1.0 27116.40 5.27 0.000 0.000 0.72-0.67 25 374 25 6.7 1.0 34142.26 5.54 0.000 0.000 0.67-0.64 31 344 31 9.0 1.0 480.62 1.51 0.000 0.000 -------------------------------------------------------------------------------------------- inf-0.64 235 2293 231 10.1 1.0 40902.14 5.64 0.045 0.055 inf-0.66 226 2125 222 10.4 1.0 42525.35 5.84 0.045 0.055 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 -1.0 0.0 1.0 1.0 0.0 1.0 1.0 2.0 RRPPROF to HKL transformation matrix: 1.0 -1.0 0.0 1.0 1.0 0.0 1.0 1.0 2.0 No constraint UB - matrix: 0.066553 0.011235 0.009528 ( 0.000067 0.000050 0.000070 ) -0.012962 0.065599 0.013276 ( 0.000046 0.000034 0.000048 ) -0.006963 -0.014784 0.066128 ( 0.000074 0.000055 0.000077 ) M - matrix: 0.004646 0.000000 0.000002 ( 0.000009 0.000005 0.000007 ) 0.000000 0.004648 0.000000 ( 0.000005 0.000005 0.000005 ) 0.000002 0.000000 0.004640 ( 0.000007 0.000005 0.000010 ) Constraint UB - matrix: 0.066553 0.011235 0.009528 ( 0.000067 0.000050 0.000070 ) -0.012962 0.065599 0.013276 ( 0.000046 0.000034 0.000048 ) -0.006963 -0.014784 0.066128 ( 0.000074 0.000055 0.000077 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) unit cell: 10.406(10) 10.404(6) 10.413(11) 90.00(6) 90.02(8) 90.00(6) V = 1127(2) unit cell: 10.4077(13) 10.4077(13) 10.4077(13) 90.0 90.0 90.0 V = 1127.4(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: (-97.000 - -72.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-318.0000 max=6134187.0000 PROFFIT INFO: signal sum lp corr: min=-244.5177 max=815648.5383 PROFFIT INFO: background sum: min=375.0000 max=4204.0000 PROFFIT INFO: background sum sig2: min=572.0000 max=4422.0000 PROFFIT INFO: num of signal pixels: min=54 max=402 PROFFIT INFO: Inet: min=-391.2284 max=1305037.7500 PROFFIT INFO: sig(Inet): min=92.1702 max=14978.3867 PROFFIT INFO: Inet/sig(Inet): min=-0.54 max=125.14 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 38 156 250 296 320 368 390 416 444 470 470 Percent 8.1 33.2 53.2 63.0 68.1 78.3 83.0 88.5 94.5 100.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 235 100.00 (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 235 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1305038- 142472 23 382389.71 70.97 100.00 140691- 5287 23 28337.25 19.65 100.00 5027- 2061 23 3036.41 8.37 91.30 2044- 1319 23 1612.53 3.67 60.87 1303- 888 23 1084.62 2.02 0.00 883- 585 23 741.70 1.85 13.04 583- 384 23 493.36 1.47 13.04 378- 127 23 271.60 0.74 0.00 124- 47 23 82.55 0.26 0.00 37- -391 28 -112.14 -0.18 0.00 ------------------------------------------------------------------------------------ 1305038- -391 235 40902.14 10.65 37.02 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 23 140369.84 20.48 78.26 1.64- 1.26 23 26335.10 13.30 65.22 1.26- 1.04 23 77405.43 20.82 65.22 1.04- 0.95 23 13557.76 4.82 21.74 0.95- 0.88 23 51461.01 15.96 47.83 0.88- 0.80 23 33709.46 9.18 30.43 0.80- 0.74 23 8116.40 3.27 13.04 0.74- 0.72 23 49124.91 14.35 30.43 0.72- 0.67 23 17195.30 5.73 21.74 0.67- 0.64 28 524.07 0.71 3.57 ------------------------------------------------------------------------------------ 6.00- 0.64 235 40902.14 10.65 37.02 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 11:59:28 2019 Sorting 235 observations 17 unique observations with > 7.00 F2/sig(F2) 235 observations in 1 runs Run # start # end # total # 1 0 24 25 Total number of frames 25 Maximum number of 17 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 235 observations in 1 runs Run # start # end # total # 1 0 12 13 Total number of frames 13 54 observations > 7.00 F2/sig(F2) 54 observations in 1 runs Run # start # end # total # 1 0 12 13 Total number of frames 13 Removing 'redundancy=1' reflections Average redundancy: 2.9 (Out of 54 removed 10 = 44, unique = 15) Not enough coverage in data - scaling will not be applied ! SCALE3 WARNING: ABSPACK failed due to insufficient data coverage PROFFIT INFO: Inet (after scale3 abspack): min=-391.2284 max=1305037.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=92.1702 max=14978.3867 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:1/25 235 reflections read from tmp file 35 reflections are rejected (10 as outliers, 25 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8+ Number of groups: 0 35 20 9 4 1 0 1 Initial Chi^2= 0.44442 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.03990 Current error model SIG(F2)^2 = 58.47*I_RAW + 0.00*I_BACK+(0.07655*)^2 Cycle 2, Chi^2= 1.01356 Current error model SIG(F2)^2 = 65.10*I_RAW + 0.00*I_BACK+(0.06412*)^2 Cycle 3, Chi^2= 1.00179 Current error model SIG(F2)^2 = 67.21*I_RAW + 0.00*I_BACK+(0.06104*)^2 Cycle 4, Chi^2= 1.00035 Current error model SIG(F2)^2 = 67.69*I_RAW + 0.00*I_BACK+(0.06012*)^2 Cycle 5, Chi^2= 1.00009 Current error model SIG(F2)^2 = 67.82*I_RAW + 0.00*I_BACK+(0.05985*)^2 Cycle 6, Chi^2= 1.00002 Current error model SIG(F2)^2 = 67.85*I_RAW + 0.00*I_BACK+(0.05977*)^2 Final Chi^2= 1.00002 Final error model SIG(F2)^2 = 67.85*I_RAW + 0.00*I_BACK+(0.05977*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1305038- 142472 23 382389.71 15.99 100.00 140691- 5287 23 28337.25 11.03 100.00 5027- 2061 23 3036.41 6.62 100.00 2044- 1319 23 1612.53 4.25 91.30 1303- 888 23 1084.62 2.99 43.48 883- 585 23 741.70 3.01 26.09 583- 384 23 493.36 2.60 17.39 378- 127 23 271.60 2.24 30.43 124- 47 23 82.55 1.17 4.35 37- -391 28 -112.14 -0.53 0.00 ------------------------------------------------------------------------------------ 1305038- -391 235 40902.14 4.82 50.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 23 140369.84 9.21 86.96 1.64- 1.26 23 26335.10 6.75 78.26 1.26- 1.04 23 77405.43 6.12 78.26 1.04- 0.95 23 13557.76 3.23 30.43 0.95- 0.88 23 51461.01 6.11 65.22 0.88- 0.80 23 33709.46 3.69 47.83 0.80- 0.74 23 8116.40 2.81 21.74 0.74- 0.72 23 49124.91 6.41 43.48 0.72- 0.67 23 17195.30 3.36 43.48 0.67- 0.64 28 524.07 1.30 14.29 ------------------------------------------------------------------------------------ 6.00- 0.64 235 40902.14 4.82 50.21 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 23 140369.84 9.21 86.96 6.00- 1.26 46 83352.47 7.98 82.61 6.00- 1.04 69 81370.12 7.36 81.16 6.00- 0.95 92 64417.03 6.33 68.48 6.00- 0.88 115 61825.83 6.28 67.83 6.00- 0.80 138 57139.77 5.85 64.49 6.00- 0.74 161 50136.43 5.42 58.39 6.00- 0.72 184 50009.99 5.54 56.52 6.00- 0.67 207 46363.91 5.30 55.07 6.00- 0.64 235 40902.14 4.82 50.21 ------------------------------------------------------------------------------------ 6.00- 0.64 235 40902.14 4.82 50.21 Scale applied to data: s=0.766261 (maximum obs:1305037.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.065; Rsigma 0.066: data 235 -> merged 97 With outlier rejection... Rint 0.059; Rsigma 0.067: data 231 -> merged 97 Rejected total: 4, method kkm 4, method Blessing 0 Completeness direct cell (a, b, c) = (10.408, 10.408, 10.408), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.636943, 6.008906 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.76 10 14 2.10 71.43 21 1.73 - 1.27 10 14 2.60 71.43 26 1.26 - 1.06 10 14 2.30 71.43 23 1.05 - 0.97 10 14 2.30 71.43 23 0.95 - 0.88 10 14 2.50 71.43 25 0.87 - 0.81 6 14 3.00 42.86 18 0.80 - 0.76 10 14 2.30 71.43 23 0.76 - 0.72 7 14 3.14 50.00 22 0.72 - 0.69 10 14 1.90 71.43 19 0.69 - 0.65 11 19 2.18 57.89 24 --------------------------------------------------------------- 7.36 - 0.65 94 145 2.38 64.83 224 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 11:59:27 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.357241 7.357848 7.360111 119.9731 119.9929 90.0132 235 Reflections read from file xs2212a.hkl 234 Reflections used for space-group determination (up to diffraction limit of 0.64A); mean (I/sigma) = 5.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 115 120 117 122 176 157 157 234 N (int>3sigma) = 0 65 71 90 64 113 103 107 150 Mean intensity = 0.0 1.0 1.1 1.6 1.0 1.2 26.8 39.1 31.5 Mean int/sigma = 0.0 3.9 4.0 5.2 3.7 4.4 5.5 5.8 5.5 Lattice type: P chosen Volume: 281.84 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 Unitcell: 7.357 7.358 7.359 60.01 60.02 89.99 Niggli form: a.a = 54.129 b.b = 54.138 c.c = 54.162 b.c = 27.068 a.c = 27.060 a.b = 0.012 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.059 CUBIC F-lattice R(int) = 0.068 [ 87] Vol = 1127.4 Cell: 10.406 10.404 10.413 90.00 90.02 90.00 Volume: 1127.37 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.043 TETRAGONAL I-lattice R(int) = 0.061 [ 15] Vol = 563.7 Cell: 7.360 7.360 10.406 89.99 89.98 89.95 Volume: 563.69 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.016 TETRAGONAL I-lattice R(int) = 0.069 [ 24] Vol = 563.7 Cell: 7.357 7.358 10.413 89.99 89.98 89.99 Volume: 563.69 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.015 ORTHORHOMBIC F-lattice R(int) = 0.070 [ 34] Vol = 1127.4 Cell: 10.406 10.404 10.413 90.00 90.02 90.00 Volume: 1127.37 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.049 ORTHORHOMBIC I-lattice R(int) = 0.075 [ 27] Vol = 563.7 Cell: 10.406 7.360 7.360 89.95 89.98 89.99 Volume: 563.69 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.013 ORTHORHOMBIC I-lattice R(int) = 0.070 [ 42] Vol = 563.7 Cell: 7.357 7.358 10.413 90.01 90.02 89.99 Volume: 563.69 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.011 MONOCLINIC I-lattice R(int) = 0.061 [ 14] Vol = 563.7 Cell: 7.359 10.404 7.362 90.00 90.04 90.01 Volume: 563.69 Matrix:-1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.019 MONOCLINIC I-lattice R(int) = 0.075 [ 11] Vol = 563.7 Cell: 7.360 10.406 7.360 90.02 90.05 89.99 Volume: 563.69 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.013 MONOCLINIC I-lattice R(int) = 0.017 [ 18] Vol = 563.7 Cell: 7.358 7.357 10.413 89.98 90.01 90.01 Volume: 563.69 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.013 MONOCLINIC I-lattice R(int) = 0.068 [ 27] Vol = 563.7 Cell: 7.357 7.358 10.413 89.99 90.02 90.01 Volume: 563.69 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.045 [ 4] Vol = 281.8 Cell: 7.357 7.358 7.359 60.01 60.02 89.99 Volume: 281.84 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 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 0 117 0 160 157 234 N (int>3sigma) = 0 0 0 0 90 0 104 103 150 Mean intensity = 0.0 0.0 0.0 0.0 1.6 0.0 37.6 26.8 31.5 Mean int/sigma = 0.0 0.0 0.0 0.0 5.2 0.0 5.6 5.5 5.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 7.054 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 1 1 19 38 N I>3s 1 1 2 31 0.1 0.1 -0.0 2.5 3.4 3.4 0.5 7.2 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 0.067 83 Fd-3m 1 1 227 C N N N N 37 2284 0.065 128 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.406338 10.403941 10.412918 90.0037 90.0195 90.0047 ZERR 1.00 0.015056 0.002458 0.027268 0.2745 0.0012 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1230647- 2127 69 66 32 2.1 137288.67 11.20 0.057 0.056 1995- 438 88 88 32 2.8 1001.15 3.28 0.158 0.162 411- -322 78 77 33 2.3 93.80 0.87 0.470 0.541 ------------------------------------------------------------------------------------------- 1230647- -322 235 231 97 2.4 39637.99 4.74 0.059 0.057 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-1.04 74 74 32 2.3 75885.19 7.01 0.043 0.042 0.062 1.02-0.77 84 82 32 2.6 26034.94 3.92 0.084 0.097 0.072 0.76-0.64 77 75 33 2.3 18746.76 3.40 0.081 0.076 0.078 ------------------------------------------------------------------------------------------------------ inf-0.64 235 231 97 2.4 39637.99 4.74 0.059 0.057 0.067 inf-0.66 226 222 93 2.4 41239.20 4.91 0.058 0.057 0.067 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-1.04 74 46 32 69.6 2.3 75885.19 11.27 0.043 0.043 1.02-0.77 82 50 32 64.0 2.6 26034.94 6.60 0.084 0.044 0.76-0.64 75 58 33 56.9 2.3 18746.76 5.58 0.081 0.049 -------------------------------------------------------------------------------------------- inf-0.64 231 154 97 63.0 2.4 39637.99 7.76 0.059 0.044 inf-0.66 222 143 93 65.0 2.4 41239.20 8.04 0.058 0.044 ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:06:15 2019) ID: 3668; threads 40; handles 811; mem 514452.00 (1204700.00)kB; time: 1w 4d 22h 17m 3s MEMORY INFO: Memory PF:70.0, Ph:532.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.4,peak PF: 700.2, WS: 470.8, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:72.0, Ph:533.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.2,peak PF: 700.2, WS: 472.6, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:06:15 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000071 0.000085 0.000140 ) 0.065981 0.091690 0.025911 ( 0.000048 0.000058 0.000095 ) 0.044418 0.058869 0.132122 ( 0.000077 0.000093 0.000154 ) 7.34808 ( 0.00628 ) 7.34732 ( 0.00610 ) 7.36303 ( 0.00880 ) 119.94370 ( 0.10487 ) 119.84600 ( 0.10678 ) 90.15964 ( 0.06931 ) V = 281.59 Selected cell (from UM rr/UM ttt/UM f): 44 7.3481 7.3473 7.3630 119.9437 119.8460 90.1596 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:06:15 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000071 0.000085 0.000140 ) 0.065981 0.091690 0.025911 ( 0.000048 0.000058 0.000095 ) 0.044418 0.058869 0.132122 ( 0.000077 0.000093 0.000154 ) M - matrix: 0.013938 0.004643 0.009284 ( 0.000015 0.000012 0.000019 ) 0.004643 0.013930 0.009277 ( 0.000012 0.000017 0.000019 ) 0.009284 0.009277 0.018560 ( 0.000019 0.000019 0.000041 ) unit cell: 7.348(6) 7.347(6) 7.363(9) 119.94(10) 119.85(11) 90.16(7) V = 281.6(5) 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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb PROFFITPEAK info: 190 peaks in the peak location table UB fit with 108 obs out of 117 (total:117,skipped:0) (92.31%) UB - matrix: 0.087042 -0.045636 0.019069 ( 0.000099 0.000074 0.000141 ) 0.065755 0.092024 0.026715 ( 0.000085 0.000063 0.000122 ) 0.044647 0.058291 0.132142 ( 0.000100 0.000074 0.000143 ) M - matrix: 0.013893 0.004681 0.009316 ( 0.000022 0.000014 0.000021 ) 0.004681 0.013949 0.009291 ( 0.000014 0.000016 0.000018 ) 0.009316 0.009291 0.018539 ( 0.000021 0.000018 0.000039 ) unit cell: 7.390(7) 7.358(7) 7.382(9) 119.93(11) 120.16(11) 90.08(8) V = 283.3(5) UB fit with 108 obs out of 117 (total:117,skipped:0) (92.31%) UB - matrix: 0.087042 -0.045636 0.019069 ( 0.000099 0.000074 0.000141 ) 0.065755 0.092024 0.026715 ( 0.000085 0.000063 0.000122 ) 0.044647 0.058291 0.132142 ( 0.000100 0.000074 0.000143 ) M - matrix: 0.013893 0.004681 0.009316 ( 0.000022 0.000014 0.000021 ) 0.004681 0.013949 0.009291 ( 0.000014 0.000016 0.000018 ) 0.009316 0.009291 0.018539 ( 0.000021 0.000018 0.000039 ) unit cell: 7.390(7) 7.358(7) 7.382(9) 119.93(11) 120.16(11) 90.08(8) V = 283.3(5) OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 UB fit with 108 obs out of 117 (total:117,skipped:0) (92.31%) UB - matrix: 0.087013 -0.045647 0.019017 ( 0.000095 0.000070 0.000135 ) 0.065790 0.092045 0.026804 ( 0.000073 0.000054 0.000104 ) 0.044698 0.058285 0.132189 ( 0.000092 0.000069 0.000132 ) M - matrix: 0.013897 0.004689 0.009327 ( 0.000021 0.000012 0.000019 ) 0.004689 0.013953 0.009304 ( 0.000012 0.000014 0.000017 ) 0.009327 0.009304 0.018554 ( 0.000019 0.000017 0.000036 ) unit cell: 7.391(7) 7.360(7) 7.383(8) 119.95(10) 120.17(11) 90.08(7) V = 283.3(5) OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 UB - matrix: 0.087031 -0.045673 0.019024 ( 0.000094 0.000070 0.000134 ) 0.065783 0.091959 0.026779 ( 0.000069 0.000051 0.000098 ) 0.044656 0.058169 0.132078 ( 0.000092 0.000068 0.000131 ) M - matrix: 0.013896 0.004672 0.009315 ( 0.000020 0.000012 0.000019 ) 0.004672 0.013926 0.009276 ( 0.000012 0.000014 0.000016 ) 0.009315 0.009276 0.018524 ( 0.000019 0.000016 0.000035 ) UB fit with 108 obs out of 117 (total:117,skipped:0) (92.31%) unit cell: 7.390(7) 7.363(6) 7.386(8) 119.93(10) 120.19(10) 90.04(7) V = 283.6(5) 117 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Run 1 Omega scan: (-97.000 - -47.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 738 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087031 -0.045673 0.019024 ( 0.000094 0.000070 0.000134 ) 0.065783 0.091959 0.026779 ( 0.000069 0.000051 0.000098 ) 0.044656 0.058169 0.132078 ( 0.000092 0.000068 0.000131 ) M - matrix: 0.013896 0.004672 0.009315 ( 0.000020 0.000012 0.000019 ) 0.004672 0.013926 0.009276 ( 0.000012 0.000014 0.000016 ) 0.009315 0.009276 0.018524 ( 0.000019 0.000016 0.000035 ) UB fit with 108 obs out of 117 (total:117,skipped:0) (92.31%) unit cell: 7.390(7) 7.363(6) 7.386(8) 119.93(10) 120.19(10) 90.04(7) V = 283.6(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 108 obs out of 117 (total:117,skipped:0) (92.31%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb 0 of 104 peaks identified as outliers and rejected 104 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 104 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 104 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.99 | 10 | 1.046 ( 0.645) | 0.889 ( 0.234) | 1.828 ( 2.683) | 2.57- 2.00 | 10 | 0.818 ( 0.081) | 0.789 ( 0.151) | 0.760 ( 0.224) | 1.99- 1.58 | 10 | 0.869 ( 0.076) | 0.912 ( 0.143) | 0.573 ( 0.196) | 1.58- 1.36 | 10 | 0.904 ( 0.080) | 0.967 ( 0.132) | 0.910 ( 0.397) | 1.36- 1.16 | 10 | 0.945 ( 0.064) | 1.023 ( 0.086) | 0.907 ( 0.458) | 1.16- 1.01 | 10 | 0.955 ( 0.091) | 1.052 ( 0.173) | 0.802 ( 0.152) | 1.01- 0.89 | 10 | 0.958 ( 0.071) | 0.995 ( 0.122) | 1.088 ( 0.431) | 0.88- 0.87 | 10 | 0.973 ( 0.092) | 1.045 ( 0.186) | 1.094 ( 0.423) | 0.87- 0.73 | 10 | 0.987 ( 0.044) | 1.016 ( 0.116) | 1.258 ( 0.427) | 0.73- 0.63 | 14 | 0.977 ( 0.046) | 0.970 ( 0.089) | 1.373 ( 0.571) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 104 | 0.944 ( 0.220) | 0.966 ( 0.166) | 1.071 ( 0.975) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 104 obs out of 104 (total:104,skipped:0) (100.00%) UB - matrix: 0.087309 -0.045834 0.019029 ( 0.000050 0.000031 0.000062 ) 0.065831 0.091897 0.026899 ( 0.000054 0.000033 0.000068 ) 0.044431 0.057865 0.131842 ( 0.000061 0.000037 0.000076 ) M - matrix: 0.013931 0.004619 0.009290 ( 0.000013 0.000008 0.000011 ) 0.004619 0.013894 0.009229 ( 0.000008 0.000008 0.000010 ) 0.009290 0.009229 0.018468 ( 0.000011 0.000010 0.000021 ) unit cell: 7.372(4) 7.362(4) 7.389(5) 119.95(6) 120.21(6) 89.85(4) V = 283.3(3) OTKP changes: 104 1 1 1 OTKP changes: 104 1 1 1 OTKP changes: 104 1 1 1 UB - matrix: 0.087284 -0.045799 0.018956 ( 0.000042 0.000026 0.000053 ) 0.065897 0.092068 0.026897 ( 0.000039 0.000024 0.000049 ) 0.044562 0.058122 0.132087 ( 0.000054 0.000033 0.000067 ) M - matrix: 0.013947 0.004660 0.009313 ( 0.000010 0.000006 0.000010 ) 0.004660 0.013952 0.009285 ( 0.000006 0.000006 0.000008 ) 0.009313 0.009285 0.018530 ( 0.000010 0.000008 0.000018 ) UB fit with 104 obs out of 104 (total:104,skipped:0) (100.00%) unit cell: 7.369(3) 7.355(3) 7.381(4) 119.99(5) 120.14(5) 89.95(3) V = 282.4(2) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - -47.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087284 -0.045799 0.018956 ( 0.000042 0.000026 0.000053 ) 0.065897 0.092068 0.026897 ( 0.000039 0.000024 0.000049 ) 0.044562 0.058122 0.132087 ( 0.000054 0.000033 0.000067 ) M - matrix: 0.013947 0.004660 0.009313 ( 0.000010 0.000006 0.000010 ) 0.004660 0.013952 0.009285 ( 0.000006 0.000006 0.000008 ) 0.009313 0.009285 0.018530 ( 0.000010 0.000008 0.000018 ) UB fit with 104 obs out of 104 (total:104,skipped:0) (100.00%) unit cell: 7.369(3) 7.355(3) 7.381(4) 119.99(5) 120.14(5) 89.95(3) V = 282.4(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 104 obs out of 104 (total:104,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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb 1 of 102 peaks identified as outliers and rejected 101 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 101 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 101 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.59 | 10 | 0.826 ( 0.091) | 0.810 ( 0.137) | 1.042 ( 0.665) | 2.38- 2.00 | 10 | 0.821 ( 0.082) | 0.799 ( 0.151) | 0.768 ( 0.320) | 1.83- 1.58 | 10 | 0.869 ( 0.080) | 0.909 ( 0.145) | 0.634 ( 0.325) | 1.58- 1.35 | 10 | 0.918 ( 0.058) | 0.987 ( 0.105) | 0.947 ( 0.379) | 1.35- 1.16 | 10 | 0.939 ( 0.075) | 1.003 ( 0.123) | 0.776 ( 0.286) | 1.16- 1.00 | 10 | 0.940 ( 0.078) | 1.021 ( 0.185) | 0.811 ( 0.171) | 1.00- 0.89 | 10 | 0.975 ( 0.079) | 1.046 ( 0.118) | 1.187 ( 0.506) | 0.89- 0.82 | 10 | 0.978 ( 0.084) | 1.069 ( 0.180) | 1.027 ( 0.443) | 0.82- 0.72 | 10 | 0.988 ( 0.039) | 0.991 ( 0.123) | 1.091 ( 0.353) | 0.72- 0.63 | 11 | 0.964 ( 0.044) | 0.984 ( 0.096) | 1.361 ( 0.544) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 101 | 0.922 ( 0.094) | 0.962 ( 0.164) | 0.968 ( 0.473) | 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 | 10 | 0.975 ( 0.038) | 1.036 ( 0.068) | 1.015 ( 0.445) | 13.3-17.1 | 10 | 0.959 ( 0.061) | 1.093 ( 0.104) | 0.861 ( 0.232) | 17.4-20.7 | 10 | 0.966 ( 0.065) | 1.056 ( 0.077) | 0.976 ( 0.498) | 21.0-25.1 | 10 | 0.962 ( 0.069) | 1.051 ( 0.094) | 0.813 ( 0.456) | 25.8-29.0 | 10 | 0.941 ( 0.095) | 1.018 ( 0.156) | 0.867 ( 0.365) | 29.0-31.4 | 10 | 0.920 ( 0.078) | 0.992 ( 0.142) | 1.021 ( 0.467) | 32.3-37.1 | 10 | 0.875 ( 0.086) | 0.884 ( 0.164) | 1.159 ( 0.597) | 37.5-39.1 | 10 | 0.844 ( 0.081) | 0.808 ( 0.120) | 1.068 ( 0.635) | 39.3-40.2 | 10 | 0.888 ( 0.106) | 0.883 ( 0.190) | 1.032 ( 0.285) | 40.6-47.6 | 11 | 0.894 ( 0.120) | 0.815 ( 0.124) | 0.879 ( 0.478) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-47.6 | 101 | 0.922 ( 0.094) | 0.962 ( 0.164) | 0.968 ( 0.473) | Fitted profile normalization line parameters e1 dimension: a=-0.0036 b=1.17 e2 dimension: a=-0.0091 b=1.35 e3 dimension: a=0.0049 b=1.02 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4846 lp-corr: 3314 Maximum peak integral for reflections I/sig<= 100 - raw: 458425 lp-corr: 293204 Maximum peak integral for reflections I/sig<= 10000 - raw: 6305074 lp-corr: 954801 PROFFITPEAK - Finished at Wed Aug 21 12:06:19 2019 PROFFITMAIN - Started at Wed Aug 21 12:06:19 2019 OTKP changes: 101 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 UB - matrix: 0.087302 -0.045810 0.018902 ( 0.000041 0.000024 0.000051 ) 0.065885 0.092066 0.026875 ( 0.000037 0.000023 0.000047 ) 0.044512 0.058108 0.132124 ( 0.000051 0.000031 0.000065 ) M - matrix: 0.013944 0.004653 0.009302 ( 0.000010 0.000006 0.000009 ) 0.004653 0.013951 0.009286 ( 0.000006 0.000006 0.000007 ) 0.009302 0.009286 0.018536 ( 0.000009 0.000007 0.000017 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 7.365(3) 7.355(3) 7.375(4) 120.00(5) 120.10(5) 89.96(3) V = 282.2(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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: (-97.000 - -47.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 719 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087302 -0.045810 0.018902 ( 0.000041 0.000024 0.000051 ) 0.065885 0.092066 0.026875 ( 0.000037 0.000023 0.000047 ) 0.044512 0.058108 0.132124 ( 0.000051 0.000031 0.000065 ) M - matrix: 0.013944 0.004653 0.009302 ( 0.000010 0.000006 0.000009 ) 0.004653 0.013951 0.009286 ( 0.000006 0.000006 0.000007 ) 0.009302 0.009286 0.018536 ( 0.000009 0.000007 0.000017 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 7.365(3) 7.355(3) 7.375(4) 120.00(5) 120.10(5) 89.96(3) V = 282.2(2) 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! 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: 0.087302 -0.045810 0.018902 ( 0.000041 0.000024 0.000051 ) 0.065885 0.092066 0.026875 ( 0.000037 0.000023 0.000047 ) 0.044512 0.058108 0.132124 ( 0.000051 0.000031 0.000065 ) M - matrix: 0.013944 0.004653 0.009302 ( 0.000010 0.000006 0.000009 ) 0.004653 0.013951 0.009286 ( 0.000006 0.000006 0.000007 ) 0.009302 0.009286 0.018536 ( 0.000009 0.000007 0.000017 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 7.365(3) 7.355(3) 7.375(4) 120.00(5) 120.10(5) 89.96(3) V = 282.2(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: 0.087302 -0.045810 0.018902 ( 0.000041 0.000024 0.000051 ) 0.065885 0.092066 0.026875 ( 0.000037 0.000023 0.000047 ) 0.044512 0.058108 0.132124 ( 0.000051 0.000031 0.000065 ) M - matrix: 0.013944 0.004653 0.009302 ( 0.000010 0.000006 0.000009 ) 0.004653 0.013951 0.009286 ( 0.000006 0.000006 0.000007 ) 0.009302 0.009286 0.018536 ( 0.000009 0.000007 0.000017 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 7.365(3) 7.355(3) 7.375(4) 120.00(5) 120.10(5) 89.96(3) V = 282.2(2) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 20 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof 483 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:06:20 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - -47.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-397.0000 max=6129297.0000 PROFFIT INFO: signal sum lp corr: min=-483.4944 max=795213.7392 PROFFIT INFO: background sum: min=367.0000 max=5968.0000 PROFFIT INFO: background sum sig2: min=480.0000 max=4800.0000 PROFFIT INFO: num of signal pixels: min=48 max=480 PROFFIT INFO: Inet: min=-773.5910 max=1272342.0000 PROFFIT INFO: sig(Inet): min=88.1674 max=17771.2422 PROFFIT INFO: Inet/sig(Inet): min=-1.23 max=206.36 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 40 163 261 304 331 382 407 425 457 480 483 Percent 8.3 33.7 54.0 62.9 68.5 79.1 84.3 88.0 94.6 99.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 483 100.00 (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 483 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1272342- 141958 48 377095.68 77.60 100.00 138792- 3622 48 31134.62 20.52 100.00 3555- 1966 48 2658.80 6.03 93.75 1964- 1233 48 1522.25 3.50 50.00 1224- 832 48 1024.02 2.16 12.50 828- 583 48 689.66 1.74 8.33 575- 399 48 489.52 1.30 8.33 398- 191 48 301.41 0.82 0.00 190- 40 48 100.82 0.34 0.00 36- -774 51 -122.16 -0.21 0.00 ------------------------------------------------------------------------------------ 1272342- -774 483 41231.00 11.31 37.06 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 48 128214.03 20.28 79.17 1.75- 1.31 48 83715.23 26.60 56.25 1.31- 1.12 48 8374.05 5.45 43.75 1.12- 0.99 48 54617.08 17.35 45.83 0.99- 0.89 48 24468.52 7.89 37.50 0.89- 0.81 48 23588.32 7.23 18.75 0.81- 0.73 48 38002.16 11.36 37.50 0.73- 0.68 48 18865.97 6.19 20.83 0.68- 0.62 48 14861.97 4.81 12.50 0.62- 0.52 51 18992.62 6.25 19.61 ------------------------------------------------------------------------------------ 6.55- 0.52 483 41231.00 11.31 37.06 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:06:20 2019 Sorting 483 observations 28 unique observations with > 7.00 F2/sig(F2) 483 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 Maximum number of 28 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 483 observations in 1 runs Run # start # end # total # 1 0 24 25 Total number of frames 25 107 observations > 7.00 F2/sig(F2) 107 observations in 1 runs Run # start # end # total # 1 0 23 24 Total number of frames 24 Removing 'redundancy=1' reflections Average redundancy: 2.5 (Out of 107 removed 49 = 58, unique = 23) 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 58 observations in 1 runs Run # start # end # total # 1 0 23 24 Total number of frames 24 Frame #4 of 24 skipped from refinement Frame #7 of 24 skipped from refinement Frame #18 of 24 skipped from refinement 3 frames need to be skipped from refinement, because of missing redundant and/or observable data 23 unique data precomputed (should be 23) 23 unique data with 58 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.5 (Out of 58 removed 0 = 58, unique = 23) 23 unique data precomputed (should be 23) 23 unique data with 58 observations RMS deviation of equivalent data = 0.29345 Rint = 0.24619 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24619, wR= 0.30649 Trying model 1 (ne=2, no=0)... Results: Rint= 0.22705, wR= 0.23104, Acormin=0.094, Acormax=0.831, Acor_av=0.377 F test: Probability=0.505, F= 1.008 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10025, wR= 0.14166, Acormin=0.130, Acormax=0.615, Acor_av=0.333 F test: Probability=1.000, F= 4.652 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: 0.26249 There are 21 active scales (one needs to be fixed) Refinement control: frame scale #22 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= 0.29345 Using Levenberg-Marquardt: 0.00010 New wR= 0.12948 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24619 with corrections 0.31182 Rint for all data: 0.26249 with corrections 0.33463 0 observations identified as outliers and rejected Cycle 2 wR= 0.12948 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= 0.06773 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24619 with corrections 0.05631 Rint for all data: 0.26249 with corrections 0.07979 0 observations identified as outliers and rejected Cycle 3 wR= 0.06773 Using Levenberg-Marquardt: 0.01000 New wR= 0.22749 Using Levenberg-Marquardt: 0.10000 New wR= 0.06442 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24619 with corrections 0.04893 Rint for all data: 0.26249 with corrections 0.07203 0 observations identified as outliers and rejected Cycle 4 wR= 0.06442 Using Levenberg-Marquardt: 0.01000 New wR= 0.09853 Using Levenberg-Marquardt: 0.10000 New wR= 0.06435 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24619 with corrections 0.04848 Rint for all data: 0.26249 with corrections 0.07156 0 observations identified as outliers and rejected Cycle 5 wR= 0.06435 Using Levenberg-Marquardt: 0.01000 New wR= 0.09714 Using Levenberg-Marquardt: 0.10000 New wR= 0.06437 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24619 with corrections 0.04847 Rint for all data: 0.26249 with corrections 0.07153 Final wR= 0.06437 Final frame scales: Min= 0.5833 Max= 1.1828 Final absorption correction factors: Amin= 0.0989 Amax= 1.2533 PROFFIT INFO: Inet (after scale3 abspack): min=-3287.9141 max=1041299.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=56.7604 max=14066.7109 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/1 frame:1/50 483 reflections read from tmp file 203 reflections are rejected (69 as outliers, 134 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 83 26 9 Initial Chi^2= 3.44338 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.72325 Current error model SIG(F2)^2 = 691.73*I_RAW + 0.00*I_BACK+(0.05529*)^2 Negative value encountered! Resetting parameters to initial values... Cycle 2, Chi^2= 1.00017 Current error model SIG(F2)^2 = 528.76*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 3, Chi^2= 1.00000 Current error model SIG(F2)^2 = 528.85*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 528.85*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1041300- 133961 48 332825.87 28.87 100.00 129247- 3571 48 24749.12 6.00 75.00 3544- 1737 48 2559.38 2.18 16.67 1721- 1187 48 1477.69 1.81 10.42 1182- 795 48 968.98 1.21 0.00 787- 530 48 645.64 1.05 0.00 527- 317 48 399.71 0.99 0.00 316- 168 48 245.66 0.79 0.00 165- 31 48 86.76 0.48 0.00 30- -3288 51 -204.00 -0.21 0.00 ------------------------------------------------------------------------------------ 1041300- -3288 483 36148.28 4.29 20.08 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 48 101197.24 13.20 56.25 1.75- 1.31 48 77059.40 7.93 35.42 1.31- 1.12 48 9677.02 2.06 18.75 1.12- 0.99 48 56746.12 5.30 20.83 0.99- 0.89 48 26187.73 2.65 10.42 0.89- 0.81 48 19437.54 2.40 8.33 0.81- 0.73 48 32716.45 3.57 20.83 0.73- 0.68 48 16484.88 2.14 8.33 0.68- 0.62 48 10090.07 1.71 8.33 0.62- 0.52 51 13313.51 2.07 13.73 ------------------------------------------------------------------------------------ 6.55- 0.52 483 36148.28 4.29 20.08 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 48 101197.24 13.20 56.25 6.55- 1.31 96 89128.32 10.57 45.83 6.55- 1.12 144 62644.55 7.73 36.81 6.55- 0.99 192 61169.95 7.12 32.81 6.55- 0.89 240 54173.50 6.23 28.33 6.55- 0.81 288 48384.17 5.59 25.00 6.55- 0.73 336 46145.93 5.30 24.40 6.55- 0.68 384 42438.30 4.91 22.40 6.55- 0.62 432 38844.05 4.55 20.83 6.55- 0.52 483 36148.28 4.29 20.08 ------------------------------------------------------------------------------------ 6.55- 0.52 483 36148.28 4.29 20.08 Scale applied to data: s=0.960338 (maximum obs:1041299.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.072; Rsigma 0.061: data 483 -> merged 261 With outlier rejection... Rint 0.057; Rsigma 0.062: data 462 -> merged 261 Rejected total: 21, method kkm 21, method Blessing 0 Completeness direct cell (a, b, c) = (6.559, 6.559, 6.559), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.516946, 6.559313 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.38 - 1.59 22 22 2.36 100.00 52 1.55 - 1.22 22 22 2.73 100.00 60 1.20 - 1.02 22 22 2.05 100.00 45 1.02 - 0.92 21 22 2.19 95.45 46 0.92 - 0.84 21 22 1.86 95.45 39 0.84 - 0.79 21 22 1.67 95.45 35 0.79 - 0.75 18 22 1.67 81.82 30 0.75 - 0.71 19 22 1.47 86.36 28 0.71 - 0.69 15 22 1.60 68.18 24 0.68 - 0.65 16 29 1.50 55.17 24 --------------------------------------------------------------- 7.38 - 0.65 197 227 1.94 86.78 383 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:06:20 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.364686 7.355356 7.375444 119.9976 120.0963 89.9576 462 Reflections read from file xs2212a.hkl 434 Reflections used for space-group determination (up to diffraction limit of 0.66A); mean (I/sigma) = 4.32 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 222 221 207 219 325 288 293 434 N (int>3sigma) = 0 15 14 23 18 26 54 55 83 Mean intensity = 0.0 1.1 1.1 1.4 1.0 1.2 33.9 38.6 35.1 Mean int/sigma = 0.0 1.2 1.3 1.7 1.2 1.4 4.0 4.8 4.3 Lattice type: P chosen Volume: 282.21 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 -1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 Unitcell: 7.355 7.355 7.365 89.96 60.05 60.04 Niggli form: a.a = 54.096 b.b = 54.101 c.c = 54.239 b.c = 0.040 a.c = 27.041 a.b = 27.019 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.245 CUBIC F-lattice R(int) = 0.233 [ 250] Vol = 1128.8 Cell: 10.405 10.420 10.412 89.84 89.93 89.95 Volume: 1128.85 Matrix: 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.085 RHOMBOHEDRAL R-lattice R(int) = 0.230 [ 158] Vol = 846.6 Cell: 7.355 7.355 18.064 90.08 90.02 119.96 Volume: 846.63 Matrix: 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.085 RHOMBOHEDRAL R-lattice R(int) = 0.335 [ 35] Vol = 846.6 Trigonal Cell: 7.355 7.355 18.064 90.08 90.02 119.96 Volume: 846.63 Matrix: 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.164 TETRAGONAL I-lattice R(int) = 0.247 [ 106] Vol = 564.4 Cell: 7.366 7.359 10.412 89.94 89.84 89.92 Volume: 564.42 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.170 ORTHORHOMBIC I-lattice R(int) = 0.253 [ 174] Vol = 564.4 Cell: 7.359 7.366 10.412 89.84 89.94 89.92 Volume: 564.42 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.141 ORTHORHOMBIC I-lattice R(int) = 0.207 [ 106] Vol = 564.4 Cell: 7.355 10.405 7.375 89.91 89.96 90.02 Volume: 564.42 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.080 MONOCLINIC I-lattice R(int) = 0.253 [ 168] Vol = 564.4 Cell: 7.366 7.359 10.412 90.06 90.16 89.92 Volume: 564.42 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.142 MONOCLINIC I-lattice R(int) = 0.055 [ 31] Vol = 564.4 Cell: 7.355 10.405 7.375 90.09 90.04 90.02 Volume: 564.42 Matrix:-1.0000 -1.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.030 MONOCLINIC I-lattice R(int) = 0.160 [ 55] Vol = 564.4 Cell: 10.405 7.355 7.375 90.04 90.09 90.02 Volume: 564.42 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.026 [ 8] Vol = 282.2 Cell: 7.355 7.355 7.365 89.96 60.05 60.04 Volume: 282.21 Matrix:-1.0000 -1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 Option [20] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 219 207 218 0 322 289 294 434 N (int>3sigma) = 0 18 23 13 0 27 59 59 83 Mean intensity = 0.0 1.0 1.4 0.9 0.0 1.1 37.4 39.1 35.1 Mean int/sigma = 0.0 1.2 1.7 1.2 0.0 1.4 4.5 4.5 4.3 Crystal system MONOCLINIC and Lattice type I selected Mean |E*E-1| = 6.139 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: c-- -a- --b N 5 15 27 N I>3s 3 0 5 3.0 0.0 2.1 5.4 0.2 2.2 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Ia (be=90) 9 A N ? Y Y 2374 341 0.100 21 Cc (be=135) 9 A N ? Y Y 2374 341 0.100 21 An (be=135) 9 A N ? Y Y 2374 341 0.100 21 I2/a (be=90) 15 C N N N N 17248 2451 0.055 30 C2/c (be=135) 15 C N N N N 17248 2451 0.055 30 A2/n (be=135) 15 C N N N N 17248 2451 0.055 31 I2/a 2/m Monoclinic (1) x, y, z (2) -x+1/2, y,-z (3) -x,-y,-z (4) x+1/2,-y, z Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in I2/a REM I2/a (#15 in standard setting) CELL 0.71073 7.355015 10.404792 7.375444 90.0862 90.0388 90.0164 ZERR 1.00 0.011811 0.006882 0.003886 0.0001 0.0744 0.0001 LATT 2 SYMM -x+1/2, y,-z 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1041300- 136255 47 44 26 1.7 333630.00 28.88 0.036 0.040 134296- 3445 43 39 26 1.5 30859.00 5.71 0.183 0.164 3413- 1799 65 57 26 2.2 2112.97 2.08 0.739 0.740 1730- 1271 57 55 26 2.1 1394.67 1.48 0.533 0.537 1269- 831 54 53 26 2.0 992.29 1.29 0.533 0.558 830- 625 52 52 26 2.0 736.51 0.94 0.711 0.704 623- 396 53 50 26 1.9 415.27 0.87 0.536 0.603 395- 264 42 42 26 1.6 324.31 0.63 0.671 0.779 262- 49 36 36 26 1.4 155.44 0.55 0.712 1.076 45- -1108 34 34 27 1.3 -136.80 -0.01 1.026 2.148 ------------------------------------------------------------------------------------------- 1041300- -1108 483 462 261 1.8 35079.19 4.11 0.057 0.060 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-1.47 74 65 27 2.4 90030.89 11.16 0.028 0.026 0.024 1.43-1.11 79 71 27 2.6 30579.45 3.44 0.050 0.060 0.064 1.09-0.94 59 55 27 2.0 50327.43 4.94 0.071 0.075 0.064 0.93-0.85 50 50 26 1.9 33931.05 3.33 0.106 0.102 0.087 0.84-0.78 45 45 27 1.7 20557.61 2.33 0.053 0.048 0.102 0.77-0.72 40 40 26 1.5 21193.43 2.65 0.087 0.111 0.102 0.72-0.68 42 42 26 1.6 18757.06 2.35 0.076 0.076 0.094 0.67-0.63 35 35 27 1.3 13546.16 2.02 0.413 0.442 0.120 0.63-0.58 34 34 27 1.3 12833.04 2.04 0.081 0.081 0.132 0.58-0.52 25 25 21 1.2 9912.45 1.71 0.255 0.255 0.129 ------------------------------------------------------------------------------------------------------ inf-0.52 483 462 261 1.8 35079.19 4.11 0.057 0.060 0.062 inf-0.65 404 383 197 1.9 39657.28 4.54 0.056 0.059 0.058 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-1.47 65 27 27 100.0 2.4 90030.89 15.79 0.028 0.018 1.43-1.11 71 27 27 100.0 2.6 30579.45 5.05 0.050 0.043 1.09-0.94 55 28 27 96.4 2.0 50327.43 6.12 0.071 0.047 0.93-0.85 50 26 26 100.0 1.9 33931.05 3.95 0.106 0.070 0.84-0.78 45 29 27 93.1 1.7 20557.61 2.86 0.053 0.093 0.77-0.72 40 31 26 83.9 1.5 21193.43 3.55 0.087 0.086 0.72-0.68 42 35 26 74.3 1.6 18757.06 3.14 0.076 0.064 0.67-0.63 35 46 27 58.7 1.3 13546.16 2.15 0.413 0.913 0.63-0.58 34 58 27 46.6 1.3 12833.04 2.44 0.081 0.094 0.58-0.52 25 116 21 18.1 1.2 9912.45 1.77 0.255 0.954 -------------------------------------------------------------------------------------------- inf-0.52 462 426 261 61.3 1.8 35079.19 5.46 0.057 0.046 inf-0.65 383 227 197 86.8 1.9 39657.28 6.12 0.056 0.044 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 -1.0 -1.0 1.0 -1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 -1.0 -1.0 1.0 -1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.020746 0.066556 -0.001844 ( 0.000021 0.000026 0.000050 ) -0.078975 -0.013091 -0.052100 ( 0.000020 0.000024 0.000046 ) -0.051310 -0.006798 0.080814 ( 0.000027 0.000032 0.000063 ) M - matrix: 0.009300 0.000002 0.000006 ( 0.000004 0.000003 0.000006 ) 0.000002 0.004647 0.000010 ( 0.000003 0.000004 0.000004 ) 0.000006 0.000010 0.009249 ( 0.000006 0.000004 0.000011 ) Constraint UB - matrix: -0.020746 0.066556 -0.001844 ( 0.000021 0.000026 0.000050 ) -0.078975 -0.013091 -0.052100 ( 0.000020 0.000024 0.000046 ) -0.051310 -0.006798 0.080814 ( 0.000027 0.000032 0.000063 ) M - matrix: 0.009295 0.000000 -0.000001 ( 0.000003 0.000000 0.000004 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000002 0.000000 ) -0.000001 0.000000 0.009313 ( 0.000004 0.000000 0.000012 ) unit cell: 7.355(3) 10.405(4) 7.375(4) 90.09(3) 90.04(4) 90.02(3) V = 564.4(4) unit cell: 7.3648(11) 10.416(2) 7.358(5) 90.0 90.00(2) 90.0 V = 564.4(4) Laue class changed... Laue class: 2/m (b-unique) - Friedel mate is equivalent Point group: 2/m (b-unique) Lattice type: I-lattice (extinction condition applied) Run 1 Omega scan: (-97.000 - -47.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-397.0000 max=6129297.0000 PROFFIT INFO: signal sum lp corr: min=-483.4944 max=795213.7392 PROFFIT INFO: background sum: min=367.0000 max=5968.0000 PROFFIT INFO: background sum sig2: min=480.0000 max=4800.0000 PROFFIT INFO: num of signal pixels: min=48 max=480 PROFFIT INFO: Inet: min=-773.5910 max=1272342.0000 PROFFIT INFO: sig(Inet): min=88.1674 max=17771.2422 PROFFIT INFO: Inet/sig(Inet): min=-1.23 max=206.36 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 80 326 522 608 662 764 814 850 914 960 966 Percent 8.3 33.7 54.0 62.9 68.5 79.1 84.3 88.0 94.6 99.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 483 100.00 (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 483 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1272342- 141958 48 377095.68 77.60 100.00 138792- 3622 48 31134.62 20.52 100.00 3555- 1966 48 2658.80 6.03 93.75 1964- 1233 48 1522.25 3.50 50.00 1224- 832 48 1024.02 2.16 12.50 828- 583 48 689.66 1.74 8.33 575- 399 48 489.52 1.30 8.33 398- 191 48 301.41 0.82 0.00 190- 40 48 100.82 0.34 0.00 36- -774 51 -122.16 -0.21 0.00 ------------------------------------------------------------------------------------ 1272342- -774 483 41231.00 11.31 37.06 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.59 48 104680.33 16.85 77.08 1.59- 1.20 48 52766.02 16.99 47.92 1.20- 1.04 48 86929.87 25.70 70.83 1.04- 0.95 48 28130.20 9.13 22.92 0.95- 0.88 48 51648.81 15.61 58.33 0.87- 0.80 48 21805.04 6.96 27.08 0.80- 0.74 48 18557.24 5.68 16.67 0.74- 0.71 48 23878.26 7.72 16.67 0.71- 0.67 48 23763.17 7.55 27.08 0.67- 0.63 51 2567.56 1.52 7.84 ------------------------------------------------------------------------------------ 6.00- 0.63 483 41231.00 11.31 37.06 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:06:20 2019 Sorting 483 observations 9 unique observations with > 7.00 F2/sig(F2) 483 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 Maximum number of 9 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 483 observations in 1 runs Run # start # end # total # 1 0 8 9 Total number of frames 9 107 observations > 7.00 F2/sig(F2) 107 observations in 1 runs Run # start # end # total # 1 0 7 8 Total number of frames 8 Removing 'redundancy=1' reflections Average redundancy: 2.1 (Out of 107 removed 86 = 21, unique = 10) Not enough coverage in data - scaling will not be applied ! SCALE3 WARNING: ABSPACK failed due to insufficient data coverage PROFFIT INFO: Inet (after scale3 abspack): min=-773.5910 max=1272342.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=88.1674 max=17771.2422 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 2, Friedel: 1 Min/max for: run:1/1 frame:1/50 483 reflections read from tmp file 417 reflections are rejected (6 as outliers, 411 as groups of 1 refl) Redundancy: 1 2 3+ Number of groups: 0 30 2 Initial Chi^2= 0.70456 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.07537 Current error model SIG(F2)^2 = 80.03*I_RAW + 0.00*I_BACK+(0.07322*)^2 Cycle 2, Chi^2= 1.00826 Current error model SIG(F2)^2 = 94.01*I_RAW + 0.00*I_BACK+(0.05145*)^2 Cycle 3, Chi^2= 0.99970 Current error model SIG(F2)^2 = 93.20*I_RAW + 0.00*I_BACK+(0.05634*)^2 Cycle 4, Chi^2= 1.00013 Current error model SIG(F2)^2 = 93.62*I_RAW + 0.00*I_BACK+(0.05498*)^2 Cycle 5, Chi^2= 0.99997 Current error model SIG(F2)^2 = 93.51*I_RAW + 0.00*I_BACK+(0.05536*)^2 Cycle 6, Chi^2= 1.00001 Current error model SIG(F2)^2 = 93.54*I_RAW + 0.00*I_BACK+(0.05526*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 93.54*I_RAW + 0.00*I_BACK+(0.05526*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1272342- 141958 48 377095.68 16.86 100.00 138792- 3622 48 31134.62 10.54 100.00 3555- 1966 48 2658.80 5.05 100.00 1964- 1233 48 1522.25 3.61 64.58 1224- 832 48 1024.02 2.71 20.83 828- 583 48 689.66 2.43 18.75 575- 399 48 489.52 2.10 12.50 398- 191 48 301.41 1.74 6.25 190- 40 48 100.82 1.19 2.08 36- -774 51 -122.16 -0.53 0.00 ------------------------------------------------------------------------------------ 1272342- -774 483 41231.00 4.54 42.24 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.59 48 104680.33 7.95 83.33 1.59- 1.20 48 52766.02 5.68 54.17 1.20- 1.04 48 86929.87 6.64 77.08 1.04- 0.95 48 28130.20 3.36 29.17 0.95- 0.88 48 51648.81 5.99 62.50 0.87- 0.80 48 21805.04 3.31 31.25 0.80- 0.74 48 18557.24 3.14 20.83 0.74- 0.71 48 23878.26 4.11 22.92 0.71- 0.67 48 23763.17 3.84 31.25 0.67- 0.63 51 2567.56 1.55 11.76 ------------------------------------------------------------------------------------ 6.00- 0.63 483 41231.00 4.54 42.24 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.59 48 104680.33 7.95 83.33 6.00- 1.20 96 78723.18 6.81 68.75 6.00- 1.04 144 81458.74 6.75 71.53 6.00- 0.95 192 68126.61 5.90 60.94 6.00- 0.88 240 64831.05 5.92 61.25 6.00- 0.80 288 57660.05 5.49 56.25 6.00- 0.74 336 52073.93 5.15 51.19 6.00- 0.71 384 48549.47 5.02 47.66 6.00- 0.67 432 45795.44 4.89 45.83 6.00- 0.63 483 41231.00 4.54 42.24 ------------------------------------------------------------------------------------ 6.00- 0.63 483 41231.00 4.54 42.24 Scale applied to data: s=0.785951 (maximum obs:1272342.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.112; Rsigma 0.064: data 483 -> merged 445 With outlier rejection... Rint 0.111; Rsigma 0.064: data 482 -> merged 445 Rejected total: 1, method kkm 1, method Blessing 0 Completeness direct cell (a, b, c) = (7.365, 10.416, 7.358), (alpha, beta, gamma) = (90.000, 89.996, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626887, 6.013506 completeness table (Laue group: I2/m (b-unique), Friedel couples are equivalent) range data theory redun '%' total 7.38 - 1.44 50 112 1.28 44.64 64 1.44 - 1.14 53 112 1.13 47.32 60 1.14 - 1.00 46 112 1.11 41.07 51 0.97 - 0.89 47 112 1.09 41.96 51 0.89 - 0.82 38 112 1.08 33.93 41 0.82 - 0.78 48 112 1.06 42.86 51 0.78 - 0.74 36 112 1.00 32.14 36 0.74 - 0.70 40 112 1.05 35.71 42 0.70 - 0.68 32 112 1.00 28.57 32 0.68 - 0.65 39 117 1.00 33.33 39 --------------------------------------------------------------- 7.38 - 0.65 429 1125 1.09 38.13 467 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:06:20 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.364686 7.355356 7.375444 119.9976 120.0963 89.9576 462 Reflections read from file xs2212a.hkl 434 Reflections used for space-group determination (up to diffraction limit of 0.66A); mean (I/sigma) = 4.32 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 222 221 207 219 325 288 293 434 N (int>3sigma) = 0 15 14 23 18 26 54 55 83 Mean intensity = 0.0 1.1 1.1 1.4 1.0 1.2 33.9 38.6 35.1 Mean int/sigma = 0.0 1.2 1.3 1.7 1.2 1.4 4.0 4.8 4.3 Lattice type: P chosen Volume: 282.21 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 -1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 Unitcell: 7.355 7.355 7.365 89.96 60.05 60.04 Niggli form: a.a = 54.096 b.b = 54.101 c.c = 54.239 b.c = 0.040 a.c = 27.041 a.b = 27.019 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.245 CUBIC F-lattice R(int) = 0.233 [ 250] Vol = 1128.8 Cell: 10.405 10.420 10.412 89.84 89.93 89.95 Volume: 1128.85 Matrix: 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.085 RHOMBOHEDRAL R-lattice R(int) = 0.230 [ 158] Vol = 846.6 Cell: 7.355 7.355 18.064 90.08 90.02 119.96 Volume: 846.63 Matrix: 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.085 RHOMBOHEDRAL R-lattice R(int) = 0.335 [ 35] Vol = 846.6 Trigonal Cell: 7.355 7.355 18.064 90.08 90.02 119.96 Volume: 846.63 Matrix: 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.164 TETRAGONAL I-lattice R(int) = 0.247 [ 106] Vol = 564.4 Cell: 7.366 7.359 10.412 89.94 89.84 89.92 Volume: 564.42 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.170 ORTHORHOMBIC I-lattice R(int) = 0.253 [ 174] Vol = 564.4 Cell: 7.359 7.366 10.412 89.84 89.94 89.92 Volume: 564.42 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.141 ORTHORHOMBIC I-lattice R(int) = 0.207 [ 106] Vol = 564.4 Cell: 7.355 10.405 7.375 89.91 89.96 90.02 Volume: 564.42 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.080 MONOCLINIC I-lattice R(int) = 0.253 [ 168] Vol = 564.4 Cell: 7.366 7.359 10.412 90.06 90.16 89.92 Volume: 564.42 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.142 MONOCLINIC I-lattice R(int) = 0.055 [ 31] Vol = 564.4 Cell: 7.355 10.405 7.375 90.09 90.04 90.02 Volume: 564.42 Matrix:-1.0000 -1.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.030 MONOCLINIC I-lattice R(int) = 0.160 [ 55] Vol = 564.4 Cell: 10.405 7.355 7.375 90.04 90.09 90.02 Volume: 564.42 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.026 [ 8] Vol = 282.2 Cell: 7.355 7.355 7.365 89.96 60.05 60.04 Volume: 282.21 Matrix:-1.0000 -1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 Option [20] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 219 207 218 0 322 289 294 434 N (int>3sigma) = 0 18 23 13 0 27 59 59 83 Mean intensity = 0.0 1.0 1.4 0.9 0.0 1.1 37.4 39.1 35.1 Mean int/sigma = 0.0 1.2 1.7 1.2 0.0 1.4 4.5 4.5 4.3 Crystal system MONOCLINIC and Lattice type I selected Mean |E*E-1| = 6.139 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: c-- -a- --b N 5 15 27 N I>3s 3 0 5 3.0 0.0 2.1 5.4 0.2 2.2 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Ia (be=90) 9 A N ? Y Y 2374 341 0.100 21 Cc (be=135) 9 A N ? Y Y 2374 341 0.100 21 An (be=135) 9 A N ? Y Y 2374 341 0.100 21 I2/a (be=90) 15 C N N N N 17248 2451 0.055 30 C2/c (be=135) 15 C N N N N 17248 2451 0.055 30 A2/n (be=135) 15 C N N N N 17248 2451 0.055 31 I2/a 2/m Monoclinic (1) x, y, z (2) -x+1/2, y,-z (3) -x,-y,-z (4) x+1/2,-y, z Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in I2/a REM I2/a (#15 in standard setting) CELL 0.71073 7.355015 10.404792 7.375444 90.0862 90.0388 90.0164 ZERR 1.00 0.011811 0.006882 0.003886 0.0001 0.0744 0.0001 LATT 2 SYMM -x+1/2, y,-z 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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: I2/m (b-unique) # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 1134047- 142359 47 47 44 1.1 382098.62 16.90 0.112 0.112 141958- 3555 52 51 44 1.2 32177.45 10.33 0.081 0.081 3552- 1901 46 46 44 1.0 2608.83 5.08 0.045 0.045 1864- 1194 52 52 44 1.2 1478.16 3.48 0.116 0.112 1176- 809 46 46 44 1.0 992.97 2.71 0.121 0.121 805- 575 48 48 44 1.1 667.83 2.35 0.329 0.329 570- 399 47 47 44 1.1 489.59 2.13 0.155 0.164 398- 191 47 47 44 1.1 299.39 1.70 0.226 0.226 190- 33 47 47 44 1.1 99.08 1.19 0.280 0.280 32- -774 51 51 49 1.0 -121.48 -0.52 1.000 2.274 ------------------------------------------------------------------------------------------- 1134047- -774 483 482 445 1.1 41306.70 4.53 0.111 0.111 Statistics vs resolution - point group symmetry: I2/m (b-unique) resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.46 58 57 44 1.3 131190.77 8.86 0.147 0.147 0.057 1.46-1.19 50 50 44 1.1 38433.18 4.86 0.060 0.060 0.062 1.16-1.02 48 48 44 1.1 48494.56 4.83 0.300 0.300 0.061 1.02-0.91 49 49 44 1.1 39361.51 4.36 0.162 0.162 0.064 0.91-0.84 48 48 44 1.1 50550.90 5.91 0.058 0.058 0.066 0.84-0.80 47 47 44 1.1 11281.92 2.56 0.116 0.116 0.083 0.80-0.74 44 44 44 1.0 20150.16 3.26 0.000 0.000 0.075 0.74-0.71 46 46 44 1.0 25042.98 4.24 0.514 0.514 0.075 0.71-0.67 44 44 44 1.0 25645.08 3.91 0.000 0.000 0.079 0.67-0.63 49 49 49 1.0 2656.84 1.53 0.000 0.000 0.184 ------------------------------------------------------------------------------------------------------ inf-0.63 483 482 445 1.1 41306.70 4.53 0.111 0.111 0.064 inf-0.66 466 465 428 1.1 42588.83 4.63 0.111 0.111 0.064 Statistics vs resolution (taking redundancy into account) - point group symmetry: I2/m (b-unique) resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.46 57 99 44 44.4 1.3 131190.77 10.38 0.147 0.040 1.46-1.19 50 96 44 45.8 1.1 38433.18 5.44 0.060 0.042 1.16-1.02 48 96 44 45.8 1.1 48494.56 4.94 0.300 0.394 1.02-0.91 49 108 44 40.7 1.1 39361.51 4.60 0.162 0.226 0.91-0.84 48 114 44 38.6 1.1 50550.90 6.45 0.058 0.045 0.84-0.80 47 104 44 42.3 1.1 11281.92 2.72 0.116 0.217 0.80-0.74 44 131 44 33.6 1.0 20150.16 3.26 0.000 0.000 0.74-0.71 46 113 44 38.9 1.0 25042.98 4.32 0.514 0.317 0.71-0.67 44 141 44 31.2 1.0 25645.08 3.91 0.000 0.000 0.67-0.63 49 253 49 19.4 1.0 2656.84 1.53 0.000 0.000 -------------------------------------------------------------------------------------------- inf-0.63 482 1270 445 35.0 1.1 41306.70 4.88 0.111 0.042 inf-0.66 465 1101 428 38.9 1.1 42588.83 4.99 0.111 0.042 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:13:03 2019) ID: 3668; threads 40; handles 809; mem 514416.00 (1204700.00)kB; time: 1w 4d 22h 23m 51s MEMORY INFO: Memory PF:71.0, Ph:526.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:502.4,peak PF: 700.2, WS: 470.7, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:73.0, Ph:528.0, V:1178.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:504.2,peak PF: 700.2, WS: 472.5, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:13:03 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000041 0.000024 0.000051 ) 0.065981 0.091690 0.025911 ( 0.000037 0.000023 0.000047 ) 0.044418 0.058869 0.132122 ( 0.000051 0.000031 0.000065 ) 7.34808 ( 0.00285 ) 7.34732 ( 0.00284 ) 7.36303 ( 0.00386 ) 119.94370 ( 0.04737 ) 119.84600 ( 0.04727 ) 90.15964 ( 0.03141 ) V = 281.59 Selected cell (from UM rr/UM ttt/UM f): 44 7.3481 7.3473 7.3630 119.9437 119.8460 90.1596 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:13:03 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000041 0.000024 0.000051 ) 0.065981 0.091690 0.025911 ( 0.000037 0.000023 0.000047 ) 0.044418 0.058869 0.132122 ( 0.000051 0.000031 0.000065 ) M - matrix: 0.013944 0.004653 0.009302 ( 0.000010 0.000006 0.000009 ) 0.004653 0.013951 0.009286 ( 0.000006 0.000006 0.000007 ) 0.009302 0.009286 0.018536 ( 0.000009 0.000007 0.000017 ) unit cell: 7.348(3) 7.347(3) 7.363(4) 119.94(5) 119.85(5) 90.16(3) V = 281.6(2) 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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb PROFFITPEAK info: 268 peaks in the peak location table UB fit with 134 obs out of 170 (total:170,skipped:0) (78.82%) UB - matrix: 0.087079 -0.045732 0.018790 ( 0.000094 0.000056 0.000115 ) 0.065675 0.092121 0.026850 ( 0.000083 0.000050 0.000102 ) 0.044372 0.058447 0.132335 ( 0.000109 0.000065 0.000134 ) M - matrix: 0.013865 0.004661 0.009272 ( 0.000022 0.000013 0.000020 ) 0.004661 0.013994 0.009349 ( 0.000013 0.000013 0.000016 ) 0.009272 0.009349 0.018586 ( 0.000020 0.000016 0.000036 ) unit cell: 7.379(6) 7.358(6) 7.370(8) 120.15(10) 119.97(10) 89.99(7) V = 282.5(5) UB fit with 134 obs out of 170 (total:170,skipped:0) (78.82%) UB - matrix: 0.087079 -0.045732 0.018790 ( 0.000094 0.000056 0.000115 ) 0.065675 0.092121 0.026850 ( 0.000083 0.000050 0.000102 ) 0.044372 0.058447 0.132335 ( 0.000109 0.000065 0.000134 ) M - matrix: 0.013865 0.004661 0.009272 ( 0.000022 0.000013 0.000020 ) 0.004661 0.013994 0.009349 ( 0.000013 0.000013 0.000016 ) 0.009272 0.009349 0.018586 ( 0.000020 0.000016 0.000036 ) unit cell: 7.379(6) 7.358(6) 7.370(8) 120.15(10) 119.97(10) 89.99(7) V = 282.5(5) OTKP changes: 65 1 1 1 OTKP changes: 65 1 1 1 OTKP changes: 65 1 1 1 UB - matrix: 0.087079 -0.045818 0.018497 ( 0.000085 0.000051 0.000103 ) 0.065363 0.092180 0.027082 ( 0.000093 0.000055 0.000113 ) 0.044980 0.057947 0.131841 ( 0.000106 0.000063 0.000129 ) M - matrix: 0.013878 0.004642 0.009311 ( 0.000021 0.000013 0.000019 ) 0.004642 0.013954 0.009289 ( 0.000013 0.000013 0.000016 ) 0.009311 0.009289 0.018458 ( 0.000019 0.000016 0.000035 ) UB fit with 152 obs out of 170 (total:170,skipped:0) (89.41%) unit cell: 7.403(6) 7.363(7) 7.421(8) 120.12(10) 120.37(10) 89.73(7) V = 284.6(5) UB fit with 152 obs out of 170 (total:170,skipped:0) (89.41%) UB - matrix: 0.087079 -0.045818 0.018497 ( 0.000085 0.000051 0.000103 ) 0.065363 0.092180 0.027082 ( 0.000093 0.000055 0.000113 ) 0.044981 0.057947 0.131841 ( 0.000106 0.000063 0.000129 ) M - matrix: 0.013878 0.004642 0.009311 ( 0.000021 0.000013 0.000019 ) 0.004642 0.013954 0.009289 ( 0.000013 0.000013 0.000016 ) 0.009311 0.009289 0.018458 ( 0.000019 0.000016 0.000035 ) unit cell: 7.403(6) 7.363(7) 7.421(8) 120.12(10) 120.37(10) 89.73(7) V = 284.6(5) OTKP changes: 67 1 1 1 OTKP changes: 67 1 1 1 OTKP changes: 67 1 1 1 UB - matrix: 0.087079 -0.045815 0.018497 ( 0.000085 0.000051 0.000103 ) 0.065363 0.092183 0.027081 ( 0.000093 0.000055 0.000113 ) 0.044984 0.057953 0.131847 ( 0.000106 0.000063 0.000129 ) M - matrix: 0.013879 0.004643 0.009312 ( 0.000021 0.000013 0.000019 ) 0.004643 0.013955 0.009290 ( 0.000013 0.000013 0.000016 ) 0.009312 0.009290 0.018459 ( 0.000019 0.000016 0.000035 ) UB fit with 152 obs out of 170 (total:170,skipped:0) (89.41%) unit cell: 7.403(6) 7.363(7) 7.420(8) 120.12(10) 120.37(10) 89.73(7) V = 284.6(5) 170 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Run 1 Omega scan: (-97.000 - -22.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1019 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087078 -0.045815 0.018497 ( 0.000085 0.000051 0.000103 ) 0.065363 0.092183 0.027081 ( 0.000093 0.000055 0.000113 ) 0.044983 0.057953 0.131847 ( 0.000106 0.000063 0.000129 ) M - matrix: 0.013879 0.004643 0.009312 ( 0.000021 0.000013 0.000019 ) 0.004643 0.013955 0.009290 ( 0.000013 0.000013 0.000016 ) 0.009312 0.009290 0.018459 ( 0.000019 0.000016 0.000035 ) UB fit with 152 obs out of 170 (total:170,skipped:0) (89.41%) unit cell: 7.403(6) 7.363(7) 7.420(8) 120.12(10) 120.37(10) 89.73(7) V = 284.6(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 153 obs out of 170 (total:170,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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb 1 of 157 peaks identified as outliers and rejected 156 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 156 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 156 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.57 | 16 | 0.839 ( 0.093) | 0.816 ( 0.132) | 1.507 ( 1.955) | 2.40- 1.76 | 16 | 0.825 ( 0.086) | 0.819 ( 0.152) | 0.748 ( 0.227) | 1.76- 1.58 | 16 | 0.860 ( 0.082) | 0.890 ( 0.130) | 0.635 ( 0.187) | 1.57- 1.35 | 16 | 0.940 ( 0.052) | 1.007 ( 0.097) | 1.039 ( 0.543) | 1.35- 1.16 | 16 | 0.955 ( 0.079) | 1.015 ( 0.143) | 0.778 ( 0.244) | 1.14- 1.01 | 16 | 0.950 ( 0.119) | 0.987 ( 0.166) | 0.917 ( 0.342) | 1.00- 0.88 | 16 | 0.968 ( 0.082) | 1.002 ( 0.145) | 1.179 ( 0.489) | 0.88- 0.79 | 16 | 0.979 ( 0.076) | 1.051 ( 0.136) | 1.076 ( 0.402) | 0.78- 0.69 | 16 | 0.976 ( 0.036) | 0.971 ( 0.109) | 1.282 ( 0.490) | 0.69- 0.63 | 12 | 0.947 ( 0.033) | 0.914 ( 0.079) | 1.429 ( 0.539) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 156 | 0.923 ( 0.097) | 0.948 ( 0.155) | 1.050 ( 0.783) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 153 obs out of 156 (total:156,skipped:0) (98.08%) UB - matrix: 0.087285 -0.045987 0.018409 ( 0.000069 0.000040 0.000078 ) 0.065258 0.092180 0.027276 ( 0.000068 0.000039 0.000077 ) 0.044983 0.057572 0.131533 ( 0.000085 0.000049 0.000096 ) M - matrix: 0.013901 0.004591 0.009304 ( 0.000017 0.000010 0.000015 ) 0.004591 0.013926 0.009240 ( 0.000010 0.000010 0.000012 ) 0.009304 0.009240 0.018384 ( 0.000015 0.000012 0.000026 ) unit cell: 7.398(5) 7.363(5) 7.439(6) 120.14(8) 120.52(8) 89.47(5) V = 284.9(4) OTKP changes: 155 1 1 1 OTKP changes: 155 1 1 1 OTKP changes: 155 1 1 1 UB - matrix: 0.087328 -0.046002 0.018240 ( 0.000067 0.000039 0.000075 ) 0.065273 0.092373 0.027250 ( 0.000071 0.000041 0.000079 ) 0.045156 0.057847 0.131801 ( 0.000078 0.000045 0.000087 ) M - matrix: 0.013926 0.004624 0.009323 ( 0.000017 0.000010 0.000014 ) 0.004624 0.013995 0.009302 ( 0.000010 0.000010 0.000011 ) 0.009323 0.009302 0.018447 ( 0.000014 0.000011 0.000023 ) UB fit with 155 obs out of 156 (total:156,skipped:0) (99.36%) unit cell: 7.390(5) 7.354(5) 7.430(6) 120.22(7) 120.45(7) 89.52(5) V = 283.8(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - -22.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1017 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087328 -0.046002 0.018240 ( 0.000067 0.000039 0.000075 ) 0.065273 0.092373 0.027250 ( 0.000071 0.000041 0.000079 ) 0.045156 0.057847 0.131801 ( 0.000078 0.000045 0.000087 ) M - matrix: 0.013926 0.004624 0.009323 ( 0.000017 0.000010 0.000014 ) 0.004624 0.013995 0.009302 ( 0.000010 0.000010 0.000011 ) 0.009323 0.009302 0.018447 ( 0.000014 0.000011 0.000023 ) UB fit with 155 obs out of 156 (total:156,skipped:0) (99.36%) unit cell: 7.390(5) 7.354(5) 7.430(6) 120.22(7) 120.45(7) 89.52(5) V = 283.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 156 obs out of 156 (total:156,skipped:0) (100.00%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb 1 of 158 peaks identified as outliers and rejected 157 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 157 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 157 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.59 | 16 | 0.921 ( 0.364) | 0.855 ( 0.191) | 1.302 ( 1.344) | 2.39- 1.75 | 16 | 0.824 ( 0.080) | 0.808 ( 0.142) | 0.702 ( 0.252) | 1.75- 1.57 | 16 | 0.865 ( 0.082) | 0.900 ( 0.126) | 0.679 ( 0.271) | 1.57- 1.35 | 16 | 0.934 ( 0.056) | 0.984 ( 0.124) | 1.065 ( 0.518) | 1.35- 1.16 | 16 | 0.967 ( 0.067) | 1.042 ( 0.115) | 0.784 ( 0.281) | 1.14- 1.00 | 16 | 0.952 ( 0.096) | 1.016 ( 0.170) | 0.926 ( 0.261) | 1.00- 0.88 | 16 | 0.956 ( 0.084) | 0.989 ( 0.131) | 1.182 ( 0.534) | 0.88- 0.78 | 16 | 0.995 ( 0.051) | 1.028 ( 0.136) | 1.102 ( 0.399) | 0.78- 0.69 | 16 | 0.983 ( 0.039) | 0.974 ( 0.105) | 1.417 ( 0.485) | 0.69- 0.63 | 13 | 0.942 ( 0.033) | 0.915 ( 0.081) | 1.362 ( 0.436) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 157 | 0.934 ( 0.143) | 0.952 ( 0.155) | 1.046 ( 0.625) | 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 | 16 | 0.975 ( 0.033) | 1.035 ( 0.067) | 1.157 ( 0.569) | 13.3-17.1 | 16 | 0.979 ( 0.067) | 1.080 ( 0.105) | 0.953 ( 0.290) | 17.2-20.7 | 16 | 0.951 ( 0.068) | 1.030 ( 0.097) | 0.889 ( 0.449) | 21.0-25.4 | 16 | 0.957 ( 0.067) | 1.010 ( 0.103) | 0.942 ( 0.510) | 25.4-29.3 | 16 | 0.945 ( 0.096) | 1.012 ( 0.156) | 0.980 ( 0.430) | 29.7-33.4 | 16 | 0.910 ( 0.087) | 0.945 ( 0.124) | 0.879 ( 0.394) | 34.0-36.9 | 16 | 0.974 ( 0.353) | 0.909 ( 0.167) | 1.526 ( 1.288) | 37.1-39.1 | 16 | 0.843 ( 0.080) | 0.795 ( 0.109) | 1.032 ( 0.501) | 39.3-41.3 | 16 | 0.905 ( 0.106) | 0.860 ( 0.163) | 1.082 ( 0.396) | 41.4-49.8 | 13 | 0.892 ( 0.103) | 0.816 ( 0.106) | 1.018 ( 0.542) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 157 | 0.934 ( 0.143) | 0.952 ( 0.155) | 1.046 ( 0.625) | Fitted profile normalization line parameters e1 dimension: a=-0.0032 b=1.14 e2 dimension: a=-0.0088 b=1.33 e3 dimension: a=0.0065 b=0.94 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 6599 lp-corr: 3607 Maximum peak integral for reflections I/sig<= 100 - raw: 459994 lp-corr: 294157 Maximum peak integral for reflections I/sig<= 10000 - raw: 6299089 lp-corr: 952658 PROFFITPEAK - Finished at Wed Aug 21 12:13:07 2019 PROFFITMAIN - Started at Wed Aug 21 12:13:07 2019 OTKP changes: 144 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 153 1 1 1 OTKP changes: 140 1 1 1 OTKP changes: 144 1 1 1 UB - matrix: 0.087307 -0.045982 0.018247 ( 0.000069 0.000039 0.000077 ) 0.065204 0.092343 0.027238 ( 0.000073 0.000041 0.000081 ) 0.045247 0.057866 0.131797 ( 0.000083 0.000047 0.000092 ) M - matrix: 0.013921 0.004625 0.009333 ( 0.000017 0.000010 0.000015 ) 0.004625 0.013990 0.009303 ( 0.000010 0.000010 0.000012 ) 0.009333 0.009303 0.018445 ( 0.000015 0.000012 0.000025 ) UB fit with 156 obs out of 157 (total:157,skipped:0) (99.36%) unit cell: 7.395(5) 7.356(5) 7.435(6) 120.23(8) 120.51(8) 89.49(5) V = 284.1(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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: (-97.000 - -22.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1005 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087307 -0.045982 0.018247 ( 0.000069 0.000039 0.000077 ) 0.065204 0.092343 0.027238 ( 0.000073 0.000041 0.000081 ) 0.045248 0.057866 0.131797 ( 0.000082 0.000046 0.000092 ) M - matrix: 0.013921 0.004625 0.009333 ( 0.000017 0.000010 0.000015 ) 0.004625 0.013990 0.009303 ( 0.000010 0.000010 0.000012 ) 0.009333 0.009303 0.018445 ( 0.000015 0.000012 0.000025 ) UB fit with 156 obs out of 157 (total:157,skipped:0) (99.36%) unit cell: 7.395(5) 7.356(5) 7.435(6) 120.23(8) 120.51(8) 89.49(5) V = 284.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 157 obs out of 157 (total:157,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118168 0.039257 0.078926 ( 0.000054 0.000030 0.000059 ) 0.000020 0.111551 0.055740 ( 0.000057 0.000032 0.000063 ) 0.000072 -0.000094 0.095443 ( 0.000090 0.000051 0.000099 ) M - matrix: 0.013964 0.004641 0.009335 ( 0.000013 0.000008 0.000012 ) 0.004641 0.013985 0.009307 ( 0.000008 0.000008 0.000009 ) 0.009335 0.009307 0.018446 ( 0.000012 0.000009 0.000022 ) UB fit with 157 obs out of 157 (total:157,skipped:0) (100.00%) unit cell: 7.379(5) 7.360(4) 7.431(9) 120.23(9) 120.41(9) 89.57(5) V = 283.6(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: 0.087301 -0.046001 0.018242 ( 0.000069 0.000039 0.000077 ) 0.065207 0.092347 0.027247 ( 0.000073 0.000041 0.000082 ) 0.045230 0.057862 0.131800 ( 0.000082 0.000046 0.000092 ) M - matrix: 0.013919 0.004623 0.009331 ( 0.000017 0.000010 0.000015 ) 0.004623 0.013992 0.009303 ( 0.000010 0.000010 0.000012 ) 0.009331 0.009303 0.018446 ( 0.000015 0.000012 0.000025 ) UB fit with 156 obs out of 157 (total:157,skipped:0) (99.36%) unit cell: 7.395(5) 7.355(5) 7.435(6) 120.23(8) 120.50(8) 89.49(5) V = 284.1(4) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 31 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof 741 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:13:08 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a Laue class: 2/m (b-unique) - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-97.000 - -22.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-802.0000 max=6122718.0000 PROFFIT INFO: signal sum lp corr: min=-546.3244 max=763543.9531 PROFFIT INFO: background sum: min=346.0000 max=5952.0000 PROFFIT INFO: background sum sig2: min=484.0000 max=5009.0000 PROFFIT INFO: num of signal pixels: min=44 max=540 PROFFIT INFO: Inet: min=-874.1191 max=1221670.3750 PROFFIT INFO: sig(Inet): min=79.2461 max=17718.8750 PROFFIT INFO: Inet/sig(Inet): min=-2.16 max=209.36 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 88 282 415 486 517 599 632 661 707 736 740 Percent 11.9 38.1 56.1 65.7 69.9 80.9 85.4 89.3 95.5 99.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 741 100.00 (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 741 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1221670- 108627 74 319159.60 69.55 100.00 107823- 3158 74 19665.04 16.87 100.00 3143- 1710 74 2348.79 5.25 86.49 1707- 1072 74 1329.97 3.19 35.14 1072- 725 74 878.25 2.05 9.46 721- 465 74 568.79 1.53 10.81 465- 284 74 369.96 1.02 1.35 284- 101 74 188.57 0.52 0.00 100- -26 74 35.26 0.12 0.00 -27- -874 74 -238.45 -0.45 0.00 ------------------------------------------------------------------------------------ 1221670- -874 740 34430.58 9.96 34.32 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.42- 1.64 74 91867.39 15.20 66.22 1.64- 1.26 74 53818.34 17.73 54.05 1.26- 1.07 74 25374.46 9.39 40.54 1.07- 0.99 74 45048.85 13.89 41.89 0.99- 0.90 74 29597.90 10.64 31.08 0.89- 0.83 74 23425.29 7.57 31.08 0.83- 0.77 74 20747.26 6.50 14.86 0.77- 0.70 74 20808.39 6.88 18.92 0.70- 0.62 74 18672.33 6.50 28.38 0.62- 0.49 74 14945.57 5.35 16.22 ------------------------------------------------------------------------------------ 6.42- 0.49 740 34430.58 9.96 34.32 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:13:08 2019 Sorting 740 observations 38 unique observations with > 7.00 F2/sig(F2) 740 observations in 1 runs Run # start # end # total # 1 0 74 75 Total number of frames 75 Maximum number of 38 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 740 observations in 1 runs Run # start # end # total # 1 0 37 38 Total number of frames 38 153 observations > 7.00 F2/sig(F2) 153 observations in 1 runs Run # start # end # total # 1 0 36 37 Total number of frames 37 Removing 'redundancy=1' reflections Average redundancy: 2.0 (Out of 153 removed 96 = 57, unique = 28) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m (b) 57 observations in 1 runs Run # start # end # total # 1 0 35 36 Total number of frames 36 Frame #6 of 36 skipped from refinement Frame #11 of 36 skipped from refinement Frame #15 of 36 skipped from refinement Frame #35 of 36 skipped from refinement 4 frames need to be skipped from refinement, because of missing redundant and/or observable data 28 unique data precomputed (should be 28) 28 unique data with 57 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.0 (Out of 57 removed 0 = 57, unique = 28) 28 unique data precomputed (should be 28) 28 unique data with 57 observations RMS deviation of equivalent data = 0.31624 Rint = 0.27681 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.27681, wR= 0.35081 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09141, wR= 0.16955, Acormin=0.057, Acormax=1.100, Acor_av=0.506 F test: Probability=1.000, F= 7.589 Trying model 2 (ne=2, no=1)... Results: Rint= 0.05702, wR= 0.13190, Acormin=0.085, Acormax=0.922, Acor_av=0.376 F test: Probability=0.968, F= 2.249 Final absorption model (ne=2, no=0): Rint= 0.09141, Acormin=0.057, Acormax=1.100, Acor_av=0.506 Combined refinement in use Rint: 0.28798 There are 32 active scales (one needs to be fixed) Refinement control: frame scale #8 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 36 pars with 666 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31624 Using Levenberg-Marquardt: 0.00010 New wR= 0.07149 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.27681 with corrections 0.06874 Rint for all data: 0.28798 with corrections 0.08678 1 observations identified as outliers and rejected Cycle 2 wR= 0.06919 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= 0.04429 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.30072 with corrections 0.03037 Rint for all data: 0.28798 with corrections 0.09860 0 observations identified as outliers and rejected Cycle 3 wR= 0.04429 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.03986 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.30072 with corrections 0.02557 Rint for all data: 0.28798 with corrections 0.10230 0 observations identified as outliers and rejected Cycle 4 wR= 0.03986 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= 0.03891 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.30072 with corrections 0.02167 Rint for all data: 0.28798 with corrections 0.09842 0 observations identified as outliers and rejected Cycle 5 wR= 0.03891 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.03921 Using Levenberg-Marquardt: 1.00000 New wR= 0.03897 Using Levenberg-Marquardt: 10.00000 New wR= 0.03892 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.30072 with corrections 0.02168 Rint for all data: 0.28798 with corrections 0.09843 Final wR= 0.03892 Final frame scales: Min= 0.4655 Max= 1.0484 Final absorption correction factors: Amin= 0.2171 Amax= 1.6907 PROFFIT INFO: Inet (after scale3 abspack): min=-2525.5586 max=1402643.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=62.4781 max=21142.4043 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 2, Friedel: 1 Min/max for: run:1/1 frame:1/75 740 reflections read from tmp file 446 reflections are rejected (41 as outliers, 405 as groups of 1 refl) Redundancy: 1 2 3+ Number of groups: 0 138 6 Initial Chi^2= 2.52868 Cycle 1, Chi^2= 0.90980 Current error model SIG(F2)^2 = 338.88*I_RAW + 30.64*I_BACK+(0.03963*)^2 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 2, Chi^2= 0.96325 Current error model SIG(F2)^2 = 441.83*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 3, Chi^2= 1.00000 Current error model SIG(F2)^2 = 425.60*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 425.60*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1402643- 68432 74 319245.56 27.35 100.00 62898- 3437 74 14095.03 5.86 77.03 3392- 1574 74 2269.30 2.16 16.22 1570- 911 74 1232.15 1.73 6.76 910- 568 74 753.55 1.23 0.00 567- 369 74 462.55 1.09 0.00 368- 217 74 290.28 0.92 0.00 214- 81 74 147.16 0.73 0.00 77- -19 74 26.85 0.23 0.00 -20- -2526 74 -341.51 -0.51 0.00 ------------------------------------------------------------------------------------ 1402643- -2526 740 33818.09 4.08 20.00 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.42- 1.64 74 103999.18 10.76 44.59 1.64- 1.26 74 59827.12 6.06 32.43 1.26- 1.07 74 27716.70 3.39 18.92 1.07- 0.99 74 48074.73 4.75 24.32 0.99- 0.90 74 28391.98 3.71 13.51 0.89- 0.83 74 25607.80 2.77 13.51 0.83- 0.77 74 15876.03 2.34 12.16 0.77- 0.70 74 12814.47 2.50 14.86 0.70- 0.62 74 9514.02 2.45 13.51 0.62- 0.49 74 6358.90 2.04 12.16 ------------------------------------------------------------------------------------ 6.42- 0.49 740 33818.09 4.08 20.00 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.42- 1.64 74 103999.18 10.76 44.59 6.42- 1.26 148 81913.15 8.41 38.51 6.42- 1.07 222 63847.67 6.74 31.98 6.42- 0.99 296 59904.43 6.24 30.07 6.42- 0.90 370 53601.94 5.74 26.76 6.42- 0.83 444 48936.25 5.24 24.55 6.42- 0.77 518 44213.36 4.83 22.78 6.42- 0.70 592 40288.50 4.54 21.79 6.42- 0.62 666 36869.11 4.30 20.87 6.42- 0.49 740 33818.09 4.08 20.00 ------------------------------------------------------------------------------------ 6.42- 0.49 740 33818.09 4.08 20.00 Scale applied to data: s=0.712939 (maximum obs:1402643.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.099; Rsigma 0.056: data 740 -> merged 554 With outlier rejection... Rint 0.040; Rsigma 0.057: data 736 -> merged 554 Rejected total: 4, method kkm 4, method Blessing 0 Completeness direct cell (a, b, c) = (7.916, 6.419, 6.876), (alpha, beta, gamma) = (90.000, 125.612, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.494551, 6.435699 completeness table (Laue group: P2/m (b-unique), Friedel couples are equivalent) range data theory redun '%' total 7.43 - 1.45 66 117 1.50 56.41 99 1.45 - 1.12 65 117 1.43 55.56 93 1.12 - 0.99 67 117 1.54 57.26 103 0.99 - 0.89 49 117 1.57 41.88 77 0.89 - 0.83 51 117 1.51 43.59 77 0.83 - 0.77 41 117 1.54 35.04 63 0.77 - 0.74 30 117 1.23 25.64 37 0.74 - 0.70 30 117 1.03 25.64 31 0.70 - 0.67 33 117 1.03 28.21 34 0.67 - 0.65 24 125 1.00 19.20 24 --------------------------------------------------------------- 7.43 - 0.65 456 1178 1.40 38.71 638 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:13:09 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.395423 7.355354 7.434835 120.2290 120.5046 89.4864 736 Reflections read from file xs2212a.hkl; mean (I/sigma) = 3.97 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 368 373 371 373 556 493 490 736 N (int>3sigma) = 0 34 32 48 34 57 97 102 146 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.9 23.5 25.3 23.5 Mean int/sigma = 0.0 1.2 1.3 1.7 1.2 1.4 3.8 4.3 4.0 Lattice type: P chosen Volume: 284.07 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 Unitcell: 7.355 7.359 7.370 90.34 119.35 119.98 Niggli form: a.a = 54.101 b.b = 54.149 c.c = 54.314 b.c = -0.322 a.c = -26.569 a.b = -27.044 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.570 CUBIC F-lattice R(int) = 0.381 [ 512] Vol = 1136.3 Cell: 10.445 10.477 10.384 90.31 89.91 90.58 Volume: 1136.27 Matrix: 1.0000 1.0000 2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.549 RHOMBOHEDRAL R-lattice R(int) = 0.347 [ 265] Vol = 852.2 Cell: 7.359 7.359 18.178 90.39 90.23 120.03 Volume: 852.20 Matrix: 1.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.549 RHOMBOHEDRAL R-lattice R(int) = 0.436 [ 62] Vol = 852.2 Trigonal Cell: 7.359 7.359 18.178 90.39 90.23 120.03 Volume: 852.20 Matrix: 1.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.417 TETRAGONAL I-lattice R(int) = 0.225 [ 189] Vol = 568.1 Cell: 7.435 7.359 10.384 89.84 89.72 89.83 Volume: 568.14 Matrix: 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.774 TETRAGONAL I-lattice R(int) = 0.225 [ 189] Vol = 568.1 Cell: 7.359 7.435 10.384 90.28 90.16 89.83 Volume: 568.14 Matrix: 1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.313 ORTHORHOMBIC I-lattice R(int) = 0.323 [ 297] Vol = 568.1 Cell: 7.359 7.435 10.384 89.72 89.84 89.83 Volume: 568.14 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.509 ORTHORHOMBIC I-lattice R(int) = 0.137 [ 305] Vol = 568.1 Cell: 7.355 10.445 7.395 89.52 89.49 89.65 Volume: 568.14 Matrix: 0.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.172 MONOCLINIC I-lattice R(int) = 0.214 [ 103] Vol = 568.1 Cell: 7.435 7.359 10.384 90.16 90.28 89.83 Volume: 568.14 Matrix: 0.0000 0.0000 1.0000 -1.0000 -1.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.549 MONOCLINIC I-lattice R(int) = 0.119 [ 221] Vol = 568.1 Cell: 7.355 7.395 10.445 90.48 90.35 89.49 Volume: 568.14 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.543 MONOCLINIC I-lattice R(int) = 0.161 [ 99] Vol = 568.1 Cell: 7.355 10.445 7.395 89.52 90.51 90.35 Volume: 568.14 Matrix: 0.0000 -1.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.481 MONOCLINIC I-lattice R(int) = 0.157 [ 117] Vol = 568.1 Cell: 7.395 7.355 10.445 89.65 90.48 90.51 Volume: 568.14 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.314 MONOCLINIC C-lattice R(int) = 0.354 [ 299] Vol = 568.1 Cell: 12.743 7.359 7.370 90.34 124.70 89.96 Volume: 568.14 Matrix: 1.0000 2.0000 1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.102 [ 18] Vol = 284.1 Cell: 7.355 7.359 7.370 90.34 119.35 119.98 Volume: 284.07 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 Option [ 7] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 370 373 371 0 557 484 499 736 N (int>3sigma) = 0 30 34 48 0 56 96 98 146 Mean intensity = 0.0 0.7 0.7 1.1 0.0 0.9 24.8 21.6 23.5 Mean int/sigma = 0.0 1.2 1.2 1.7 0.0 1.4 4.0 3.8 4.0 Crystal system TETRAGONAL and Lattice type I selected Mean |E*E-1| = 3.903 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41/43 a-- -c- --d N 1 18 61 37 N I>3s 0 0 17 0 -0.0 -0.0 1.8 -0.1 -0.3 0.1 2.6 -0.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) I4(1)/amd 1 1 141 C N N N N 41 526 0.298 368 I4(1)/amd 4/mmm Tetragonal (1) x, y, z (2) -x+1/2,-y, z+1/2 (3) -y+1/4, x+3/4, z+1/4 (4) y+1/4,-x+1/4, z+3/4 (5) -x+1/2, y,-z+1/2 (6) x,-y,-z (7) y+1/4, x+3/4,-z+1/4 (8) -y+1/4,-x+1/4,-z+3/4 (9) -x,-y,-z (10) x+1/2, y,-z+1/2 (11) y+3/4,-x+1/4,-z+3/4 (12) -y+3/4, x+3/4,-z+1/4 (13) x+1/2,-y, z+1/2 (14) -x, y, z (15) -y+3/4,-x+1/4, z+3/4 (16) y+3/4, x+3/4, z+1/4 Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in I4(1)/amd REM I4(1)/amd (#141 in standard setting) CELL 0.71073 7.434835 7.359428 10.383560 89.8404 89.7193 89.8268 ZERR 1.00 0.005937 0.019497 0.011990 0.0005 0.0012 0.1275 LATT 2 SYMM -x+1/2,-y, z+1/2 SYMM -y+1/4, x+3/4, z+1/4 SYMM y+1/4,-x+1/4, z+3/4 SYMM -x+1/2, y,-z+1/2 SYMM x,-y,-z SYMM y+1/4, x+3/4,-z+1/4 SYMM -y+1/4,-x+1/4,-z+3/4 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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: P2/m (b-unique) # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 1402643- 89152 73 72 55 1.3 316402.99 26.66 0.020 0.020 68432- 3220 71 71 55 1.3 15010.88 5.84 0.332 0.339 3132- 1560 84 81 55 1.5 2168.60 2.11 0.574 0.576 1556- 905 87 87 55 1.6 1223.65 1.66 0.469 0.480 904- 623 80 80 55 1.5 766.53 1.16 0.525 0.533 619- 383 67 67 55 1.2 489.35 1.10 0.679 0.695 381- 243 74 74 55 1.3 311.24 0.80 0.703 0.830 243- 102 69 69 55 1.3 168.03 0.72 0.677 0.770 101- -11 64 64 55 1.2 44.97 0.30 0.900 1.501 -11- -2526 71 71 59 1.2 -305.32 -0.35 0.926 1.436 ------------------------------------------------------------------------------------------- 1402643- -2526 740 736 554 1.3 32933.20 3.97 0.040 0.040 Statistics vs resolution - point group symmetry: P2/m (b-unique) resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.56 87 83 55 1.5 95494.98 9.83 0.022 0.022 0.021 1.54-1.22 76 76 55 1.4 49180.93 4.91 0.058 0.057 0.045 1.22-1.05 84 84 55 1.5 39720.55 4.22 0.052 0.052 0.061 1.04-0.93 84 84 55 1.5 32002.65 3.44 0.044 0.044 0.082 0.93-0.85 90 90 55 1.6 35869.90 4.23 0.028 0.028 0.081 0.85-0.78 81 81 55 1.5 6973.01 1.27 0.129 0.131 0.176 0.78-0.71 68 68 55 1.2 22318.58 3.57 0.065 0.065 0.083 0.71-0.67 56 56 55 1.0 4870.15 1.68 0.244 0.244 0.152 0.67-0.60 55 55 55 1.0 9720.42 2.47 0.000 0.000 0.094 0.60-0.49 59 59 59 1.0 7324.33 2.22 0.000 0.000 0.111 ------------------------------------------------------------------------------------------------------ inf-0.49 740 736 554 1.3 32933.20 3.97 0.040 0.040 0.057 inf-0.65 642 638 456 1.4 36634.05 4.20 0.040 0.040 0.056 Statistics vs resolution (taking redundancy into account) - point group symmetry: P2/m (b-unique) resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.56 83 98 55 56.1 1.5 95494.98 10.73 0.022 0.018 1.54-1.22 76 95 55 57.9 1.4 49180.93 5.68 0.058 0.043 1.22-1.05 84 104 55 52.9 1.5 39720.55 4.66 0.052 0.061 1.04-0.93 84 109 55 50.5 1.5 32002.65 4.29 0.044 0.051 0.93-0.85 90 123 55 44.7 1.6 35869.90 4.48 0.028 0.055 0.85-0.78 81 148 55 37.2 1.5 6973.01 1.59 0.129 0.125 0.78-0.71 68 206 55 26.7 1.2 22318.58 4.08 0.065 0.070 0.71-0.67 56 207 55 26.6 1.0 4870.15 1.70 0.244 0.714 0.67-0.60 55 368 55 14.9 1.0 9720.42 2.47 0.000 0.000 0.60-0.49 59 1097 59 5.4 1.0 7324.33 2.22 0.000 0.000 -------------------------------------------------------------------------------------------- inf-0.49 736 2567 554 21.6 1.3 32933.20 4.41 0.040 0.048 inf-0.65 638 1171 456 38.9 1.4 36634.05 4.71 0.040 0.048 Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 0.0 0.0 -1.0 1.0 1.0 1.0 1.0 -1.0 0.0 RRPPROF to HKL transformation matrix: 0.0 0.0 -1.0 1.0 1.0 1.0 1.0 -1.0 0.0 No constraint UB - matrix: 0.002271 0.020665 0.066626 ( 0.000062 0.000038 0.000031 ) 0.051628 0.078812 -0.013504 ( 0.000068 0.000041 0.000033 ) -0.080273 0.051543 -0.006325 ( 0.000081 0.000049 0.000040 ) M - matrix: 0.009114 -0.000022 -0.000038 ( 0.000015 0.000008 0.000006 ) -0.000022 0.009295 -0.000013 ( 0.000008 0.000008 0.000004 ) -0.000038 -0.000013 0.004661 ( 0.000006 0.000004 0.000004 ) Constraint UB - matrix: 0.002271 0.020665 0.066626 ( 0.000062 0.000038 0.000031 ) 0.051628 0.078812 -0.013504 ( 0.000068 0.000041 0.000033 ) -0.080273 0.051543 -0.006325 ( 0.000081 0.000049 0.000040 ) M - matrix: 0.009293 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.009293 0.000000 ( 0.000000 0.000003 0.000000 ) 0.000000 0.000000 0.004649 ( 0.000000 0.000000 0.000002 ) unit cell: 7.430(5) 7.357(4) 10.389(5) 89.88(4) 89.66(4) 89.86(5) V = 567.9(6) unit cell: 7.3783(11) 7.3783(11) 10.431(2) 90.0 90.0 90.0 V = 567.87(17) Laue class changed... Laue class: 4/mmm - Friedel mate is equivalent Point group: 4/mmm Lattice type: I-lattice (extinction condition applied) Run 1 Omega scan: (-97.000 - -22.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-802.0000 max=6122718.0000 PROFFIT INFO: signal sum lp corr: min=-546.3244 max=763543.9531 PROFFIT INFO: background sum: min=346.0000 max=5952.0000 PROFFIT INFO: background sum sig2: min=484.0000 max=5009.0000 PROFFIT INFO: num of signal pixels: min=44 max=540 PROFFIT INFO: Inet: min=-874.1191 max=1221670.3750 PROFFIT INFO: sig(Inet): min=79.2461 max=17718.8750 PROFFIT INFO: Inet/sig(Inet): min=-2.16 max=209.36 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 176 564 830 972 1034 1198 1264 1322 1414 1472 1480 Percent 11.9 38.1 56.1 65.7 69.9 80.9 85.4 89.3 95.5 99.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 741 100.00 (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 741 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1221670- 108627 74 319159.60 69.55 100.00 107823- 3158 74 19665.04 16.87 100.00 3143- 1710 74 2348.79 5.25 86.49 1707- 1072 74 1329.97 3.19 35.14 1072- 725 74 878.25 2.05 9.46 721- 465 74 568.79 1.53 10.81 465- 284 74 369.96 1.02 1.35 284- 101 74 188.57 0.52 0.00 100- -26 74 35.26 0.12 0.00 -27- -874 74 -238.45 -0.45 0.00 ------------------------------------------------------------------------------------ 1221670- -874 740 34430.58 9.96 34.32 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.59 74 73789.75 13.05 70.27 1.59- 1.23 74 46646.62 15.38 45.95 1.23- 1.05 74 71896.48 21.21 63.51 1.05- 0.94 74 25745.58 8.23 20.27 0.94- 0.86 74 51475.67 15.79 56.76 0.86- 0.80 74 10377.55 4.20 20.27 0.80- 0.75 74 16857.41 5.40 16.22 0.75- 0.71 74 23812.03 7.91 18.92 0.71- 0.67 74 21177.02 7.04 24.32 0.67- 0.63 74 2527.64 1.43 6.76 ------------------------------------------------------------------------------------ 6.01- 0.63 740 34430.58 9.96 34.32 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:13:09 2019 Sorting 740 observations 49 unique observations with > 7.00 F2/sig(F2) 740 observations in 1 runs Run # start # end # total # 1 0 74 75 Total number of frames 75 Maximum number of 49 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 740 observations in 1 runs Run # start # end # total # 1 0 37 38 Total number of frames 38 153 observations > 7.00 F2/sig(F2) 153 observations in 1 runs Run # start # end # total # 1 0 36 37 Total number of frames 37 Removing 'redundancy=1' reflections Average redundancy: 2.5 (Out of 153 removed 34 = 119, unique = 47) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m2/m2/m 119 observations in 1 runs Run # start # end # total # 1 0 36 37 Total number of frames 37 47 unique data precomputed (should be 47) 47 unique data with 119 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.5 (Out of 119 removed 0 = 119, unique = 47) 47 unique data precomputed (should be 47) 47 unique data with 119 observations RMS deviation of equivalent data = 0.13848 Rint = 0.12727 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.12727, wR= 0.14177 Trying model 1 (ne=2, no=0)... Results: Rint= 0.10260, wR= 0.11229, Acormin=0.530, Acormax=1.324, Acor_av=0.734 F test: Probability=0.931, F= 1.432 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08931, wR= 0.09623, Acormin=0.424, Acormax=1.299, Acor_av=0.722 F test: Probability=0.991, F= 1.805 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07058, wR= 0.07778, Acormin=0.478, Acormax=0.999, Acor_av=0.719 F test: Probability=0.924, F= 1.451 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06661, wR= 0.07356, Acormin=0.433, Acormax=1.090, Acor_av=0.717 F test: Probability=0.950, F= 1.545 Trying model 5 (ne=4, no=3)... Results: Rint= 0.04704, wR= 0.04894, Acormin=0.496, Acormax=1.429, Acor_av=0.845 F test: Probability=1.000, F= 2.703 Final absorption model (ne=4, no=3): Rint= 0.04704, Acormin=0.496, Acormax=1.429, Acor_av=0.845 Combined refinement in use Rint: 0.13051 There are 37 active scales (one needs to be fixed) Refinement control: frame scale #4 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 60 pars with 1830 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13848 Using Levenberg-Marquardt: 0.00010 New wR= 0.02830 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.12727 with corrections 0.03040 Rint for all data: 0.13051 with corrections 0.03553 0 observations identified as outliers and rejected Cycle 2 wR= 0.02830 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= 0.02561 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.12727 with corrections 0.02441 Rint for all data: 0.13051 with corrections 0.02961 0 observations identified as outliers and rejected Cycle 3 wR= 0.02561 Using Levenberg-Marquardt: 0.00100 New wR= 0.02493 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.12727 with corrections 0.02348 Rint for all data: 0.13051 with corrections 0.02873 0 observations identified as outliers and rejected Cycle 4 wR= 0.02493 Using Levenberg-Marquardt: 0.00010 New wR= 0.02450 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.12727 with corrections 0.02266 Rint for all data: 0.13051 with corrections 0.02789 0 observations identified as outliers and rejected Cycle 5 wR= 0.02450 Using Levenberg-Marquardt: 0.00001 New wR= 0.02449 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.12727 with corrections 0.02201 Rint for all data: 0.13051 with corrections 0.02725 Final wR= 0.02449 Final frame scales: Min= 0.9772 Max= 1.1339 Final absorption correction factors: Amin= 0.2327 Amax= 1.7548 PROFFIT INFO: Inet (after scale3 abspack): min=-869.2220 max=1079789.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=81.6956 max=29262.4863 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 6, Friedel: 1 Min/max for: run:1/1 frame:1/75 740 reflections read from tmp file 105 reflections are rejected (8 as outliers, 97 as groups of 1 refl) Redundancy: 1 2 3 4 5 6+ Number of groups: 0 154 64 26 5 1 Initial Chi^2= 0.69442 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.08250 Current error model SIG(F2)^2 = 120.50*I_RAW + 0.00*I_BACK+(0.02604*)^2 Cycle 2, Chi^2= 1.00109 Current error model SIG(F2)^2 = 134.77*I_RAW + 0.00*I_BACK+(0.01841*)^2 Cycle 3, Chi^2= 1.00004 Current error model SIG(F2)^2 = 135.08*I_RAW + 0.00*I_BACK+(0.01812*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 135.07*I_RAW + 0.00*I_BACK+(0.01815*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 135.07*I_RAW + 0.00*I_BACK+(0.01815*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1079789- 104540 74 312020.43 31.71 100.00 101059- 3089 74 20591.82 9.96 100.00 3035- 1642 74 2266.27 4.22 83.78 1640- 977 74 1259.87 2.86 36.49 976- 678 74 829.73 2.07 5.41 671- 439 74 542.48 1.75 1.35 439- 259 74 356.43 1.72 8.11 259- 105 74 184.00 1.25 2.70 102- -28 74 34.84 0.35 0.00 -29- -869 74 -240.96 -0.92 0.00 ------------------------------------------------------------------------------------ 1079789- -869 740 33784.49 5.50 33.78 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.59 74 78845.72 9.28 72.97 1.59- 1.23 74 47904.98 7.20 43.24 1.23- 1.05 74 69206.88 9.35 60.81 1.05- 0.94 74 25229.46 4.22 21.62 0.94- 0.86 74 47142.24 8.46 56.76 0.86- 0.80 74 9831.57 2.66 18.92 0.80- 0.75 74 14892.63 3.48 13.51 0.75- 0.71 74 22927.24 4.81 18.92 0.71- 0.67 74 19263.60 4.25 27.03 0.67- 0.63 74 2600.61 1.24 4.05 ------------------------------------------------------------------------------------ 6.01- 0.63 740 33784.49 5.50 33.78 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.59 74 78845.72 9.28 72.97 6.01- 1.23 148 63375.35 8.24 58.11 6.01- 1.05 222 65319.19 8.61 59.01 6.01- 0.94 296 55296.76 7.51 49.66 6.01- 0.86 370 53665.86 7.70 51.08 6.01- 0.80 444 46360.14 6.86 45.72 6.01- 0.75 518 41864.78 6.38 41.12 6.01- 0.71 592 39497.59 6.18 38.34 6.01- 0.67 666 37249.37 5.97 37.09 6.01- 0.63 740 33784.49 5.50 33.78 ------------------------------------------------------------------------------------ 6.01- 0.63 740 33784.49 5.50 33.78 Scale applied to data: s=0.926106 (maximum obs:1079789.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.027; Rsigma 0.039: data 740 -> merged 347 With outlier rejection... Rint 0.026; Rsigma 0.039: data 726 -> merged 347 Rejected total: 14, method kkm 14, method Blessing 0 Completeness direct cell (a, b, c) = (7.378, 7.378, 10.431), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627908, 6.023735 completeness table (Laue group: I4/mmm (tetra-c), Friedel couples are equivalent) range data theory redun '%' total 7.43 - 1.59 29 34 2.59 85.29 75 1.59 - 1.20 32 34 2.41 94.12 77 1.20 - 1.02 33 34 2.27 97.06 75 1.02 - 0.91 34 34 2.29 100.00 78 0.91 - 0.85 34 34 2.12 100.00 72 0.85 - 0.80 34 34 2.15 100.00 73 0.80 - 0.75 33 34 1.91 97.06 63 0.75 - 0.72 31 34 1.97 91.18 61 0.72 - 0.68 31 34 1.81 91.18 56 0.68 - 0.65 35 41 1.97 85.37 69 --------------------------------------------------------------- 7.43 - 0.65 326 347 2.14 93.95 699 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:13:09 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.395423 7.355354 7.434835 120.2290 120.5046 89.4864 736 Reflections read from file xs2212a.hkl; mean (I/sigma) = 3.97 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 368 373 371 373 556 493 490 736 N (int>3sigma) = 0 34 32 48 34 57 97 102 146 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.9 23.5 25.3 23.5 Mean int/sigma = 0.0 1.2 1.3 1.7 1.2 1.4 3.8 4.3 4.0 Lattice type: P chosen Volume: 284.07 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 Unitcell: 7.355 7.359 7.370 90.34 119.35 119.98 Niggli form: a.a = 54.101 b.b = 54.149 c.c = 54.314 b.c = -0.322 a.c = -26.569 a.b = -27.044 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.570 CUBIC F-lattice R(int) = 0.381 [ 512] Vol = 1136.3 Cell: 10.445 10.477 10.384 90.31 89.91 90.58 Volume: 1136.27 Matrix: 1.0000 1.0000 2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.549 RHOMBOHEDRAL R-lattice R(int) = 0.347 [ 265] Vol = 852.2 Cell: 7.359 7.359 18.178 90.39 90.23 120.03 Volume: 852.20 Matrix: 1.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.549 RHOMBOHEDRAL R-lattice R(int) = 0.436 [ 62] Vol = 852.2 Trigonal Cell: 7.359 7.359 18.178 90.39 90.23 120.03 Volume: 852.20 Matrix: 1.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.417 TETRAGONAL I-lattice R(int) = 0.225 [ 189] Vol = 568.1 Cell: 7.435 7.359 10.384 89.84 89.72 89.83 Volume: 568.14 Matrix: 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.774 TETRAGONAL I-lattice R(int) = 0.225 [ 189] Vol = 568.1 Cell: 7.359 7.435 10.384 90.28 90.16 89.83 Volume: 568.14 Matrix: 1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.313 ORTHORHOMBIC I-lattice R(int) = 0.323 [ 297] Vol = 568.1 Cell: 7.359 7.435 10.384 89.72 89.84 89.83 Volume: 568.14 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.509 ORTHORHOMBIC I-lattice R(int) = 0.137 [ 305] Vol = 568.1 Cell: 7.355 10.445 7.395 89.52 89.49 89.65 Volume: 568.14 Matrix: 0.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.172 MONOCLINIC I-lattice R(int) = 0.214 [ 103] Vol = 568.1 Cell: 7.435 7.359 10.384 90.16 90.28 89.83 Volume: 568.14 Matrix: 0.0000 0.0000 1.0000 -1.0000 -1.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.549 MONOCLINIC I-lattice R(int) = 0.119 [ 221] Vol = 568.1 Cell: 7.355 7.395 10.445 90.48 90.35 89.49 Volume: 568.14 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.543 MONOCLINIC I-lattice R(int) = 0.161 [ 99] Vol = 568.1 Cell: 7.355 10.445 7.395 89.52 90.51 90.35 Volume: 568.14 Matrix: 0.0000 -1.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.481 MONOCLINIC I-lattice R(int) = 0.157 [ 117] Vol = 568.1 Cell: 7.395 7.355 10.445 89.65 90.48 90.51 Volume: 568.14 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.314 MONOCLINIC C-lattice R(int) = 0.354 [ 299] Vol = 568.1 Cell: 12.743 7.359 7.370 90.34 124.70 89.96 Volume: 568.14 Matrix: 1.0000 2.0000 1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.102 [ 18] Vol = 284.1 Cell: 7.355 7.359 7.370 90.34 119.35 119.98 Volume: 284.07 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 Option [ 7] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 370 373 371 0 557 484 499 736 N (int>3sigma) = 0 30 34 48 0 56 96 98 146 Mean intensity = 0.0 0.7 0.7 1.1 0.0 0.9 24.8 21.6 23.5 Mean int/sigma = 0.0 1.2 1.2 1.7 0.0 1.4 4.0 3.8 4.0 Crystal system TETRAGONAL and Lattice type I selected Mean |E*E-1| = 3.903 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41/43 a-- -c- --d N 1 18 61 37 N I>3s 0 0 17 0 -0.0 -0.0 1.8 -0.1 -0.3 0.1 2.6 -0.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) I4(1)/amd 1 1 141 C N N N N 41 526 0.298 368 I4(1)/amd 4/mmm Tetragonal (1) x, y, z (2) -x+1/2,-y, z+1/2 (3) -y+1/4, x+3/4, z+1/4 (4) y+1/4,-x+1/4, z+3/4 (5) -x+1/2, y,-z+1/2 (6) x,-y,-z (7) y+1/4, x+3/4,-z+1/4 (8) -y+1/4,-x+1/4,-z+3/4 (9) -x,-y,-z (10) x+1/2, y,-z+1/2 (11) y+3/4,-x+1/4,-z+3/4 (12) -y+3/4, x+3/4,-z+1/4 (13) x+1/2,-y, z+1/2 (14) -x, y, z (15) -y+3/4,-x+1/4, z+3/4 (16) y+3/4, x+3/4, z+1/4 Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in I4(1)/amd REM I4(1)/amd (#141 in standard setting) CELL 0.71073 7.434835 7.359428 10.383560 89.8404 89.7193 89.8268 ZERR 1.00 0.005937 0.019497 0.011990 0.0005 0.0012 0.1275 LATT 2 SYMM -x+1/2,-y, z+1/2 SYMM -y+1/4, x+3/4, z+1/4 SYMM y+1/4,-x+1/4, z+3/4 SYMM -x+1/2, y,-z+1/2 SYMM x,-y,-z SYMM y+1/4, x+3/4,-z+1/4 SYMM -y+1/4,-x+1/4,-z+3/4 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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: I4/mmm # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 1042722- 125563 62 62 34 1.8 350161.81 34.24 0.020 0.020 121016- 3867 74 72 34 2.1 39597.03 12.29 0.033 0.034 3363- 1773 84 80 34 2.4 2365.73 4.34 0.136 0.141 1665- 974 79 79 34 2.3 1262.55 2.70 0.188 0.179 974- 671 67 66 34 1.9 814.90 2.04 0.205 0.212 666- 423 80 80 34 2.4 534.25 1.70 0.358 0.369 409- 277 79 77 34 2.3 359.47 1.51 0.431 0.478 269- 128 75 74 34 2.2 202.92 1.21 0.526 0.655 125- -21 70 68 34 2.0 55.44 0.45 0.772 1.401 -25- -869 70 68 41 1.7 -189.20 -0.67 0.631 0.764 ------------------------------------------------------------------------------------------- 1042722- -869 740 726 347 2.1 34407.91 5.55 0.026 0.026 Statistics vs resolution - point group symmetry: I4/mmm resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.46 91 87 34 2.6 106453.75 11.68 0.023 0.021 0.023 1.46-1.15 81 80 34 2.4 51679.58 7.76 0.015 0.014 0.030 1.15-1.01 85 80 34 2.4 13943.34 3.56 0.014 0.011 0.049 1.01-0.91 78 78 34 2.3 30435.13 5.23 0.025 0.026 0.038 0.89-0.84 70 70 34 2.1 42592.66 7.59 0.029 0.033 0.043 0.84-0.78 70 69 34 2.0 24052.80 4.80 0.055 0.053 0.052 0.78-0.74 66 65 34 1.9 2309.97 1.60 0.270 0.271 0.168 0.73-0.71 68 66 34 1.9 25839.26 5.28 0.037 0.036 0.060 0.70-0.67 64 64 34 1.9 22015.41 4.68 0.035 0.036 0.070 0.67-0.63 67 67 41 1.6 2824.39 1.28 0.389 0.419 0.181 ------------------------------------------------------------------------------------------------------ inf-0.63 740 726 347 2.1 34407.91 5.55 0.026 0.026 0.039 inf-0.66 711 697 325 2.1 35597.72 5.72 0.026 0.026 0.038 Statistics vs resolution (taking redundancy into account) - point group symmetry: I4/mmm resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.46 87 39 34 87.2 2.6 106453.75 19.32 0.023 0.015 1.46-1.15 80 36 34 94.4 2.4 51679.58 11.56 0.015 0.019 1.15-1.01 80 35 34 97.1 2.4 13943.34 5.29 0.014 0.031 1.01-0.91 78 34 34 100.0 2.3 30435.13 7.55 0.025 0.026 0.89-0.84 70 34 34 100.0 2.1 42592.66 11.68 0.029 0.027 0.84-0.78 69 34 34 100.0 2.0 24052.80 6.50 0.055 0.036 0.78-0.74 65 37 34 91.9 1.9 2309.97 2.11 0.270 0.409 0.73-0.71 66 35 34 97.1 1.9 25839.26 7.47 0.037 0.043 0.70-0.67 64 40 34 85.0 1.9 22015.41 6.62 0.035 0.047 0.67-0.63 67 69 41 59.4 1.6 2824.39 1.60 0.389 0.544 -------------------------------------------------------------------------------------------- inf-0.63 726 393 347 88.3 2.1 34407.91 8.33 0.026 0.026 inf-0.66 697 344 325 94.5 2.1 35597.72 8.61 0.026 0.026 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:19:52 2019) ID: 3668; threads 40; handles 811; mem 514252.00 (1204700.00)kB; time: 1w 4d 22h 30m 40s MEMORY INFO: Memory PF:73.0, Ph:524.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.2,peak PF: 700.2, WS: 470.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:75.0, Ph:525.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.0,peak PF: 700.2, WS: 472.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:19:52 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000069 0.000039 0.000077 ) 0.065981 0.091690 0.025911 ( 0.000073 0.000041 0.000082 ) 0.044418 0.058869 0.132122 ( 0.000082 0.000046 0.000092 ) 7.34808 ( 0.00484 ) 7.34732 ( 0.00501 ) 7.36303 ( 0.00583 ) 119.94370 ( 0.07693 ) 119.84600 ( 0.07547 ) 90.15964 ( 0.05429 ) V = 281.59 Selected cell (from UM rr/UM ttt/UM f): 44 7.3481 7.3473 7.3630 119.9437 119.8460 90.1596 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:19:52 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000069 0.000039 0.000077 ) 0.065981 0.091690 0.025911 ( 0.000073 0.000041 0.000082 ) 0.044418 0.058869 0.132122 ( 0.000082 0.000046 0.000092 ) M - matrix: 0.013919 0.004623 0.009330 ( 0.000017 0.000010 0.000015 ) 0.004623 0.013992 0.009303 ( 0.000010 0.000010 0.000012 ) 0.009330 0.009303 0.018447 ( 0.000015 0.000012 0.000025 ) unit cell: 7.348(5) 7.347(5) 7.363(6) 119.94(8) 119.85(7) 90.16(5) V = 281.6(3) 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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb PROFFITPEAK info: 369 peaks in the peak location table UB fit with 149 obs out of 225 (total:225,skipped:0) (66.22%) UB - matrix: 0.087053 -0.045748 0.018695 ( 0.000091 0.000054 0.000110 ) 0.065636 0.092116 0.026769 ( 0.000094 0.000056 0.000114 ) 0.044281 0.058458 0.132317 ( 0.000118 0.000070 0.000143 ) M - matrix: 0.013847 0.004652 0.009244 ( 0.000023 0.000014 0.000021 ) 0.004652 0.013996 0.009346 ( 0.000014 0.000014 0.000017 ) 0.009244 0.009346 0.018574 ( 0.000021 0.000017 0.000039 ) unit cell: 7.376(7) 7.358(7) 7.366(9) 120.17(11) 119.89(11) 90.01(7) V = 282.5(5) UB fit with 149 obs out of 225 (total:225,skipped:0) (66.22%) UB - matrix: 0.087053 -0.045748 0.018695 ( 0.000091 0.000054 0.000110 ) 0.065636 0.092116 0.026769 ( 0.000094 0.000056 0.000114 ) 0.044281 0.058458 0.132317 ( 0.000118 0.000070 0.000143 ) M - matrix: 0.013847 0.004652 0.009244 ( 0.000023 0.000014 0.000021 ) 0.004652 0.013996 0.009346 ( 0.000014 0.000014 0.000017 ) 0.009244 0.009346 0.018574 ( 0.000021 0.000017 0.000039 ) unit cell: 7.376(7) 7.358(7) 7.366(9) 120.17(11) 119.89(11) 90.01(7) V = 282.5(5) OTKP changes: 78 1 1 1 OTKP changes: 78 1 1 1 OTKP changes: 78 1 1 1 UB - matrix: 0.087153 -0.045927 0.018002 ( 0.000092 0.000057 0.000102 ) 0.065032 0.092284 0.027258 ( 0.000097 0.000061 0.000108 ) 0.045309 0.057861 0.131817 ( 0.000108 0.000067 0.000120 ) M - matrix: 0.013878 0.004620 0.009314 ( 0.000023 0.000014 0.000019 ) 0.004620 0.013974 0.009316 ( 0.000014 0.000015 0.000016 ) 0.009314 0.009316 0.018443 ( 0.000019 0.000016 0.000032 ) UB fit with 185 obs out of 225 (total:225,skipped:0) (82.22%) unit cell: 7.406(7) 7.368(7) 7.441(8) 120.31(10) 120.48(10) 89.48(7) V = 285.0(5) UB fit with 185 obs out of 225 (total:225,skipped:0) (82.22%) UB - matrix: 0.087137 -0.045931 0.017947 ( 0.000094 0.000059 0.000104 ) 0.065022 0.092284 0.027215 ( 0.000098 0.000061 0.000108 ) 0.045390 0.057861 0.131851 ( 0.000108 0.000067 0.000118 ) M - matrix: 0.013881 0.004624 0.009318 ( 0.000023 0.000014 0.000019 ) 0.004624 0.013974 0.009316 ( 0.000014 0.000015 0.000016 ) 0.009318 0.009316 0.018447 ( 0.000019 0.000016 0.000032 ) unit cell: 7.406(7) 7.368(7) 7.440(8) 120.30(10) 120.48(10) 89.49(7) V = 284.9(5) OTKP changes: 86 1 1 1 OTKP changes: 86 1 1 1 OTKP changes: 86 1 1 1 UB - matrix: 0.087215 -0.045979 0.017843 ( 0.000094 0.000060 0.000105 ) 0.064968 0.092325 0.027266 ( 0.000095 0.000060 0.000105 ) 0.045507 0.057856 0.131894 ( 0.000109 0.000070 0.000122 ) M - matrix: 0.013898 0.004621 0.009330 ( 0.000023 0.000014 0.000019 ) 0.004621 0.013985 0.009328 ( 0.000014 0.000015 0.000016 ) 0.009330 0.009328 0.018458 ( 0.000019 0.000016 0.000033 ) UB fit with 190 obs out of 225 (total:225,skipped:0) (84.44%) unit cell: 7.402(7) 7.367(7) 7.443(8) 120.35(10) 120.52(10) 89.42(7) V = 284.7(5) 225 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Run 1 Omega scan: (-97.000 - 3.000,100 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1296 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087215 -0.045979 0.017843 ( 0.000094 0.000060 0.000105 ) 0.064971 0.092325 0.027268 ( 0.000095 0.000060 0.000105 ) 0.045510 0.057856 0.131897 ( 0.000109 0.000070 0.000122 ) M - matrix: 0.013899 0.004621 0.009330 ( 0.000023 0.000014 0.000019 ) 0.004621 0.013985 0.009328 ( 0.000014 0.000015 0.000016 ) 0.009330 0.009328 0.018459 ( 0.000019 0.000016 0.000033 ) UB fit with 190 obs out of 225 (total:225,skipped:0) (84.44%) unit cell: 7.402(7) 7.367(7) 7.443(8) 120.35(10) 120.52(10) 89.42(7) V = 284.7(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 199 obs out of 225 (total:225,skipped:0) (88.44%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb 0 of 211 peaks identified as outliers and rejected 211 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 211 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 211 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.97 | 21 | 0.997 ( 0.547) | 0.872 ( 0.223) | 1.606 ( 2.201) | 2.61- 1.76 | 21 | 0.838 ( 0.088) | 0.833 ( 0.148) | 0.808 ( 0.425) | 1.76- 1.58 | 21 | 0.839 ( 0.091) | 0.864 ( 0.145) | 0.649 ( 0.254) | 1.57- 1.36 | 21 | 0.940 ( 0.058) | 1.007 ( 0.108) | 1.132 ( 0.657) | 1.35- 1.16 | 21 | 0.945 ( 0.079) | 1.023 ( 0.131) | 1.014 ( 0.712) | 1.16- 1.01 | 21 | 0.918 ( 0.087) | 0.968 ( 0.185) | 0.835 ( 0.224) | 1.01- 0.88 | 21 | 0.965 ( 0.068) | 0.991 ( 0.125) | 1.225 ( 0.503) | 0.88- 0.79 | 21 | 0.992 ( 0.055) | 1.050 ( 0.133) | 1.186 ( 0.395) | 0.79- 0.70 | 21 | 0.981 ( 0.042) | 0.959 ( 0.109) | 1.217 ( 0.472) | 0.69- 0.63 | 22 | 0.944 ( 0.037) | 0.929 ( 0.098) | 1.286 ( 0.473) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 211 | 0.936 ( 0.193) | 0.949 ( 0.161) | 1.097 ( 0.872) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 191 obs out of 211 (total:211,skipped:0) (90.52%) UB - matrix: 0.087359 -0.046162 0.017737 ( 0.000088 0.000055 0.000091 ) 0.064849 0.092233 0.027350 ( 0.000082 0.000050 0.000084 ) 0.045290 0.057619 0.131768 ( 0.000097 0.000060 0.000100 ) M - matrix: 0.013888 0.004558 0.009291 ( 0.000021 0.000012 0.000017 ) 0.004558 0.013958 0.009296 ( 0.000012 0.000013 0.000013 ) 0.009291 0.009296 0.018425 ( 0.000017 0.000013 0.000027 ) unit cell: 7.394(6) 7.369(6) 7.444(6) 120.43(9) 120.52(9) 89.20(6) V = 284.7(4) OTKP changes: 193 1 1 1 OTKP changes: 193 1 1 1 OTKP changes: 193 1 1 1 UB - matrix: 0.087459 -0.046068 0.017511 ( 0.000094 0.000059 0.000093 ) 0.064687 0.092368 0.027223 ( 0.000089 0.000056 0.000088 ) 0.045570 0.057917 0.132120 ( 0.000100 0.000063 0.000100 ) M - matrix: 0.013910 0.004585 0.009313 ( 0.000022 0.000013 0.000017 ) 0.004585 0.014008 0.009360 ( 0.000013 0.000014 0.000014 ) 0.009313 0.009360 0.018504 ( 0.000017 0.000014 0.000027 ) UB fit with 199 obs out of 211 (total:211,skipped:0) (94.31%) unit cell: 7.387(6) 7.366(6) 7.435(7) 120.53(9) 120.46(9) 89.22(7) V = 283.7(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 3.000,100 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1290 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087459 -0.046068 0.017511 ( 0.000094 0.000059 0.000093 ) 0.064687 0.092368 0.027223 ( 0.000089 0.000056 0.000088 ) 0.045570 0.057917 0.132120 ( 0.000100 0.000063 0.000100 ) M - matrix: 0.013910 0.004585 0.009313 ( 0.000022 0.000013 0.000017 ) 0.004585 0.014008 0.009360 ( 0.000013 0.000014 0.000014 ) 0.009313 0.009360 0.018504 ( 0.000017 0.000014 0.000027 ) UB fit with 199 obs out of 211 (total:211,skipped:0) (94.31%) unit cell: 7.387(6) 7.366(6) 7.435(7) 120.53(9) 120.46(9) 89.22(7) V = 283.7(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 211 (total:211,skipped:0) (97.16%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb 0 of 208 peaks identified as outliers and rejected 208 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 208 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 208 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.99 | 21 | 0.995 ( 0.545) | 0.843 ( 0.183) | 1.634 ( 2.376) | 2.60- 1.76 | 21 | 0.827 ( 0.090) | 0.820 ( 0.153) | 0.751 ( 0.317) | 1.75- 1.56 | 21 | 0.854 ( 0.086) | 0.882 ( 0.143) | 0.662 ( 0.230) | 1.56- 1.35 | 21 | 0.934 ( 0.070) | 1.003 ( 0.122) | 1.103 ( 0.542) | 1.35- 1.16 | 21 | 0.963 ( 0.068) | 1.030 ( 0.121) | 0.927 ( 0.382) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.961 ( 0.182) | 0.964 ( 0.396) | 1.00- 0.88 | 21 | 0.975 ( 0.069) | 1.002 ( 0.127) | 1.238 ( 0.488) | 0.88- 0.78 | 21 | 0.978 ( 0.051) | 1.019 ( 0.139) | 1.121 ( 0.357) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.952 ( 0.102) | 1.287 ( 0.503) | 0.69- 0.63 | 19 | 0.945 ( 0.035) | 0.927 ( 0.107) | 1.292 ( 0.456) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 208 | 0.939 ( 0.192) | 0.944 ( 0.157) | 1.096 ( 0.895) | 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 | 21 | 0.974 ( 0.042) | 1.055 ( 0.063) | 1.144 ( 0.489) | 12.7-16.5 | 21 | 1.078 ( 0.434) | 1.094 ( 0.118) | 1.513 ( 2.172) | 16.5-20.6 | 21 | 0.942 ( 0.067) | 1.011 ( 0.098) | 1.031 ( 0.538) | 20.6-25.0 | 21 | 0.966 ( 0.062) | 1.021 ( 0.106) | 1.044 ( 0.485) | 25.0-29.2 | 21 | 0.944 ( 0.083) | 1.002 ( 0.133) | 0.985 ( 0.428) | 29.2-33.4 | 21 | 0.894 ( 0.088) | 0.925 ( 0.130) | 0.804 ( 0.386) | 33.6-36.9 | 21 | 0.947 ( 0.299) | 0.854 ( 0.115) | 1.364 ( 1.065) | 36.9-39.0 | 21 | 0.851 ( 0.083) | 0.809 ( 0.129) | 1.009 ( 0.449) | 39.1-41.7 | 21 | 0.903 ( 0.098) | 0.857 ( 0.166) | 1.102 ( 0.408) | 41.9-49.8 | 19 | 0.882 ( 0.116) | 0.801 ( 0.120) | 0.950 ( 0.515) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 208 | 0.939 ( 0.192) | 0.944 ( 0.157) | 1.096 ( 0.895) | Fitted profile normalization line parameters e1 dimension: a=-0.0032 b=1.13 e2 dimension: a=-0.0087 b=1.33 e3 dimension: a=0.0022 b=1.01 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4854 lp-corr: 3597 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 315077 Maximum peak integral for reflections I/sig<= 10000 - raw: 6305075 lp-corr: 953958 PROFFITPEAK - Finished at Wed Aug 21 12:19:57 2019 PROFFITMAIN - Started at Wed Aug 21 12:19:57 2019 OTKP changes: 161 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 172 1 1 1 OTKP changes: 142 1 1 1 OTKP changes: 159 1 1 1 UB - matrix: 0.087368 -0.046095 0.017672 ( 0.000090 0.000055 0.000088 ) 0.064875 0.092370 0.027310 ( 0.000082 0.000050 0.000081 ) 0.045418 0.057866 0.132015 ( 0.000099 0.000061 0.000098 ) M - matrix: 0.013905 0.004593 0.009312 ( 0.000021 0.000012 0.000017 ) 0.004593 0.014005 0.009347 ( 0.000012 0.000013 0.000013 ) 0.009312 0.009347 0.018486 ( 0.000017 0.000013 0.000026 ) UB fit with 194 obs out of 208 (total:208,skipped:0) (93.27%) unit cell: 7.390(6) 7.364(6) 7.435(6) 120.47(9) 120.45(9) 89.29(6) V = 283.9(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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: (-97.000 - 3.000,100 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1275 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087402 -0.046099 0.017653 ( 0.000089 0.000055 0.000087 ) 0.064865 0.092371 0.027331 ( 0.000080 0.000049 0.000079 ) 0.045519 0.057853 0.132017 ( 0.000097 0.000060 0.000095 ) M - matrix: 0.013918 0.004596 0.009325 ( 0.000021 0.000012 0.000017 ) 0.004596 0.014004 0.009348 ( 0.000012 0.000013 0.000013 ) 0.009325 0.009348 0.018487 ( 0.000017 0.000013 0.000026 ) UB fit with 195 obs out of 208 (total:208,skipped:0) (93.75%) unit cell: 7.390(6) 7.365(6) 7.439(6) 120.47(9) 120.50(9) 89.26(6) V = 283.9(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 202 obs out of 208 (total:208,skipped:0) (97.12%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118230 0.039123 0.078975 ( 0.000076 0.000047 0.000071 ) 0.000086 0.111671 0.056268 ( 0.000074 0.000046 0.000069 ) 0.000002 -0.000072 0.095567 ( 0.000093 0.000057 0.000087 ) M - matrix: 0.013978 0.004635 0.009342 ( 0.000018 0.000010 0.000014 ) 0.004635 0.014001 0.009366 ( 0.000010 0.000011 0.000011 ) 0.009342 0.009366 0.018536 ( 0.000014 0.000011 0.000022 ) UB fit with 205 obs out of 208 (total:208,skipped:0) (98.56%) unit cell: 7.367(5) 7.368(5) 7.419(8) 120.43(9) 120.34(9) 89.47(6) V = 282.8(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 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\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: 0.087389 -0.046122 0.017650 ( 0.000088 0.000054 0.000087 ) 0.064871 0.092376 0.027337 ( 0.000081 0.000050 0.000079 ) 0.045493 0.057852 0.132030 ( 0.000097 0.000060 0.000095 ) M - matrix: 0.013915 0.004594 0.009322 ( 0.000021 0.000012 0.000017 ) 0.004594 0.014007 0.009349 ( 0.000012 0.000013 0.000013 ) 0.009322 0.009349 0.018491 ( 0.000017 0.000013 0.000026 ) UB fit with 195 obs out of 208 (total:208,skipped:0) (93.75%) unit cell: 7.390(6) 7.364(6) 7.437(6) 120.47(9) 120.49(9) 89.26(6) V = 283.8(4) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 40 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof 986 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:19:59 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a Laue class: 4/m - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-97.000 - 3.000,100 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-631.0000 max=6112769.0000 PROFFIT INFO: signal sum lp corr: min=-491.5011 max=766620.7055 PROFFIT INFO: background sum: min=224.0000 max=5938.0000 PROFFIT INFO: background sum sig2: min=503.0000 max=4982.0000 PROFFIT INFO: num of signal pixels: min=50 max=497 PROFFIT INFO: Inet: min=-786.4017 max=1226593.1250 PROFFIT INFO: sig(Inet): min=63.5019 max=17638.9316 PROFFIT INFO: Inet/sig(Inet): min=-1.71 max=193.53 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 120 384 561 645 687 791 841 882 945 981 986 Percent 12.2 38.9 56.9 65.4 69.7 80.2 85.3 89.5 95.8 99.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 986 100.00 (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 986 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1226593- 108045 98 309341.85 68.28 100.00 107613- 3163 98 20724.69 16.99 100.00 3151- 1748 98 2415.71 5.88 92.86 1738- 1054 98 1346.40 3.40 37.76 1051- 720 98 867.52 1.92 10.20 717- 454 98 577.18 1.43 5.10 454- 271 98 349.95 1.01 2.04 270- 88 98 170.97 0.48 0.00 87- -28 98 34.56 0.13 0.00 -28- -786 104 -201.15 -0.38 0.00 ------------------------------------------------------------------------------------ 1226593- -786 986 33357.31 9.85 34.58 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.87- 1.82 98 89109.37 15.84 67.35 1.82- 1.34 98 61970.19 20.03 54.08 1.34- 1.13 98 14351.58 7.18 48.98 1.13- 0.99 98 50116.34 15.46 41.84 0.99- 0.90 98 34414.78 11.01 31.63 0.90- 0.82 98 15605.37 5.33 18.37 0.82- 0.74 98 20189.06 6.93 28.57 0.74- 0.68 98 22640.32 7.45 21.43 0.68- 0.62 98 14241.67 4.96 16.33 0.62- 0.49 104 12228.01 4.63 18.27 ------------------------------------------------------------------------------------ 6.87- 0.49 986 33357.31 9.85 34.58 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:19:59 2019 Sorting 986 observations 50 unique observations with > 7.00 F2/sig(F2) 986 observations in 1 runs Run # start # end # total # 1 0 99 100 Total number of frames 100 Maximum number of 50 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 986 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 49 50 Total number of frames 50 Frame #25 of 50 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 216 removed 96 = 120, 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): 4/m 120 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 Frame #25 of 50 skipped from refinement Frame #32 of 50 skipped from refinement Frame #48 of 50 skipped from refinement Frame #49 of 50 skipped from refinement 4 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 120 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.4 (Out of 120 removed 0 = 120, unique = 49) 49 unique data precomputed (should be 49) 49 unique data with 120 observations RMS deviation of equivalent data = 0.28598 Rint = 0.23755 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.23755, wR= 0.31415 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11958, wR= 0.18933, Acormin=0.139, Acormax=1.653, Acor_av=0.524 F test: Probability=1.000, F= 3.668 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12772, wR= 0.19298, Acormin=0.159, Acormax=1.462, Acor_av=0.457 F test: Probability=0.000, F= 0.837 Trying model 3 (ne=4, no=0)... Results: Rint= 0.14951, wR= 0.13490, Acormin=-0.022, Acormax=1.982, Acor_av=0.268 F test: Probability=0.000, F= 0.553 Trying model 4 (ne=4, no=1)... Results: Rint= 0.14655, wR= 0.13387, Acormin=0.023, Acormax=2.009, Acor_av=0.281 F test: Probability=0.000, F= 0.545 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08497, wR= 0.11879, Acormin=0.056, Acormax=1.222, Acor_av=0.298 F test: Probability=0.892, F= 1.410 Final absorption model (ne=2, no=0): Rint= 0.11958, Acormin=0.139, Acormax=1.653, Acor_av=0.524 Combined refinement in use Rint: 0.24967 There are 46 active scales (one needs to be fixed) Refinement control: frame scale #20 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 50 pars with 1275 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.28598 Using Levenberg-Marquardt: 0.00010 New wR= 0.15246 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.22829 Rint for all data: 0.24967 with corrections 0.33769 0 observations identified as outliers and rejected Cycle 2 wR= 0.15246 Using Levenberg-Marquardt: 0.00001 New wR= 0.12711 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.12527 Rint for all data: 0.24967 with corrections 0.56758 0 observations identified as outliers and rejected Cycle 3 wR= 0.12711 Using Levenberg-Marquardt: 0.00000 New wR= 0.10599 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.10392 Rint for all data: 0.24967 with corrections 0.13480 0 observations identified as outliers and rejected Cycle 4 wR= 0.10599 Using Levenberg-Marquardt: 0.00000 New wR= 0.32180 Using Levenberg-Marquardt: 0.00000 New wR= 0.31871 Using Levenberg-Marquardt: 0.00001 New wR= 0.28983 Using Levenberg-Marquardt: 0.00010 New wR= 0.15425 Using Levenberg-Marquardt: 0.00100 New wR= 0.10581 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.09695 Rint for all data: 0.24967 with corrections 0.11925 0 observations identified as outliers and rejected Cycle 5 wR= 0.10581 Using Levenberg-Marquardt: 0.00010 New wR= 0.18536 Using Levenberg-Marquardt: 0.00100 New wR= 0.12723 Using Levenberg-Marquardt: 0.01000 New wR= 0.10255 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.09126 Rint for all data: 0.24967 with corrections 0.11631 0 observations identified as outliers and rejected Final wR= 0.10255 Final frame scales: Min= 0.7881 Max= 1.2249 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics There are 46 active scales (one needs to be fixed) Refinement control: frame scale #20 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 45 pars with 1035 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.74988 Using Levenberg-Marquardt: 0.00010 New wR= 0.23225 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.18910 Rint for all data: 0.24967 with corrections 0.20276 0 observations identified as outliers and rejected Cycle 2 wR= 0.23225 Using Levenberg-Marquardt: 0.00001 New wR= 0.22121 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.21133 Rint for all data: 0.24967 with corrections 0.22353 0 observations identified as outliers and rejected Cycle 3 wR= 0.22121 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= 0.26047 Using Levenberg-Marquardt: 0.10000 New wR= 0.21513 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.20687 Rint for all data: 0.24967 with corrections 0.21934 0 observations identified as outliers and rejected Cycle 4 wR= 0.21513 Using Levenberg-Marquardt: 0.01000 New wR= 0.21361 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.19774 Rint for all data: 0.24967 with corrections 0.21053 0 observations identified as outliers and rejected Cycle 5 wR= 0.21361 Using Levenberg-Marquardt: 0.00100 New wR= 0.26043 Using Levenberg-Marquardt: 0.01000 New wR= 0.21463 Using Levenberg-Marquardt: 0.10000 New wR= 0.21362 There are 3 clusters with unrefined scales (size 1-2) Rint for refined data: 0.23755 with corrections 0.19727 Rint for all data: 0.24967 with corrections 0.21000 Final wR= 0.21362 Final frame scales: Min= 1.0000 Max= 2.7631 PROFFIT INFO: Inet (after scale3 abspack): min=-890.0134 max=1111048.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=56.2959 max=20197.0371 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 5, Friedel: 1 Min/max for: run:1/1 frame:1/100 986 reflections read from tmp file 512 reflections are rejected (122 as outliers, 390 as groups of 1 refl) Redundancy: 1 2 3 4 5+ Number of groups: 0 172 28 9 2 Initial Chi^2= 3.39374 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.75364 Current error model SIG(F2)^2 = 656.50*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 494.77*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 494.77*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1111048- 98239 98 309539.03 24.96 100.00 95578- 3457 98 18862.20 5.37 74.49 3452- 1719 98 2373.78 2.24 13.27 1718- 1047 98 1330.46 1.55 3.06 1046- 684 98 855.22 1.16 0.00 680- 435 98 549.48 0.97 0.00 434- 249 98 335.69 0.84 1.02 248- 82 98 165.85 0.59 0.00 82- -27 98 33.99 0.25 0.00 -29- -890 104 -198.10 -0.43 0.00 ------------------------------------------------------------------------------------ 1111048- -890 986 33180.40 3.73 19.07 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.87- 1.82 98 84352.97 9.97 43.88 1.82- 1.34 98 66818.77 6.27 28.57 1.34- 1.13 98 18950.30 2.51 21.43 1.13- 0.99 98 47804.73 4.91 19.39 0.99- 0.90 98 32436.43 3.60 16.33 0.90- 0.82 98 14848.58 1.92 8.16 0.82- 0.74 98 21073.94 2.36 13.27 0.74- 0.68 98 23198.39 2.53 14.29 0.68- 0.62 98 12589.76 1.66 11.22 0.62- 0.49 104 11083.04 1.66 14.42 ------------------------------------------------------------------------------------ 6.87- 0.49 986 33180.40 3.73 19.07 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.87- 1.82 98 84352.97 9.97 43.88 6.87- 1.34 196 75585.87 8.12 36.22 6.87- 1.13 294 56707.35 6.25 31.29 6.87- 0.99 392 54481.69 5.92 28.32 6.87- 0.90 490 50072.64 5.45 25.92 6.87- 0.82 588 44201.96 4.86 22.96 6.87- 0.74 686 40897.96 4.51 21.57 6.87- 0.68 784 38685.51 4.26 20.66 6.87- 0.62 882 35785.99 3.97 19.61 6.87- 0.49 986 33180.40 3.73 19.07 ------------------------------------------------------------------------------------ 6.87- 0.49 986 33180.40 3.73 19.07 Scale applied to data: s=0.900050 (maximum obs:1111048.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.210; Rsigma 0.062: data 986 -> merged 625 With outlier rejection... Rint 0.174; Rsigma 0.065: data 950 -> merged 625 Rejected total: 36, method kkm 36, method Blessing 0 Completeness direct cell (a, b, c) = (6.887, 6.887, 5.984), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.486653, 6.886782 completeness table (Laue group: P4/m (tetra-c), Friedel couples are equivalent) range data theory redun '%' total 7.42 - 1.47 58 59 2.48 98.31 144 1.46 - 1.13 59 59 2.02 100.00 119 1.13 - 0.98 59 59 1.76 100.00 104 0.98 - 0.90 57 59 1.61 96.61 92 0.90 - 0.82 55 59 1.47 93.22 81 0.82 - 0.77 51 59 1.41 86.44 72 0.77 - 0.74 47 59 1.26 79.66 59 0.74 - 0.70 46 59 1.22 77.97 56 0.70 - 0.67 32 59 1.22 54.24 39 0.67 - 0.65 34 59 1.18 57.63 40 --------------------------------------------------------------- 7.42 - 0.65 498 590 1.62 84.41 806 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:19:59 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.389630 7.363616 7.437053 120.4722 120.4926 89.2579 950 Reflections read from file xs2212a.hkl 514 Reflections used for space-group determination (up to diffraction limit of 0.82A); mean (I/sigma) = 4.97 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 251 265 260 254 388 343 353 514 N (int>3sigma) = 0 28 27 47 28 51 78 77 114 Mean intensity = 0.0 1.2 1.3 1.9 1.3 1.5 42.7 41.1 40.6 Mean int/sigma = 0.0 1.5 1.5 2.2 1.5 1.8 5.1 5.2 5.0 Lattice type: P chosen Volume: 283.81 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.348 7.358 7.364 119.97 119.27 90.38 Niggli form: a.a = 53.989 b.b = 54.143 c.c = 54.223 b.c = -27.067 a.c = -26.451 a.b = -0.356 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 6] err= 0.524 TETRAGONAL I-lattice R(int) = 0.140 [ 244] Vol = 567.6 Cell: 7.364 7.437 10.364 89.91 89.80 89.64 Volume: 567.62 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.672 TETRAGONAL I-lattice R(int) = 0.189 [ 249] Vol = 567.6 Cell: 7.348 7.358 10.499 90.26 89.46 90.38 Volume: 567.62 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.584 TETRAGONAL I-lattice R(int) = 0.140 [ 244] Vol = 567.6 Cell: 7.437 7.364 10.364 90.20 89.91 90.36 Volume: 567.62 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.734 ORTHORHOMBIC F-lattice R(int) = 0.159 [ 228] Vol = 1135.2 Cell: 10.364 10.433 10.499 89.44 90.20 89.92 Volume: 1135.24 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.404 ORTHORHOMBIC I-lattice R(int) = 0.152 [ 258] Vol = 567.6 Cell: 10.364 7.437 7.364 89.64 89.80 89.91 Volume: 567.62 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.650 ORTHORHOMBIC I-lattice R(int) = 0.169 [ 272] Vol = 567.6 Cell: 7.348 7.358 10.499 89.74 90.54 90.38 Volume: 567.62 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.280 MONOCLINIC I-lattice R(int) = 0.078 [ 120] Vol = 567.6 Cell: 7.364 10.364 7.437 89.91 90.36 90.20 Volume: 567.62 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.599 MONOCLINIC I-lattice R(int) = 0.173 [ 126] Vol = 567.6 Cell: 7.364 10.433 7.390 90.34 90.74 89.54 Volume: 567.62 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.221 MONOCLINIC I-lattice R(int) = 0.078 [ 120] Vol = 567.6 Cell: 7.437 10.364 7.364 90.20 90.36 89.91 Volume: 567.62 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.356 MONOCLINIC I-lattice R(int) = 0.161 [ 211] Vol = 567.6 Cell: 7.348 7.358 10.499 90.26 90.54 89.62 Volume: 567.62 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.405 MONOCLINIC I-lattice R(int) = 0.196 [ 118] Vol = 567.6 Cell: 7.348 10.499 7.358 90.26 90.38 89.46 Volume: 567.62 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.750 MONOCLINIC I-lattice R(int) = 0.196 [ 118] Vol = 567.6 Cell: 7.348 10.499 7.358 89.74 90.38 90.54 Volume: 567.62 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.137 [ 29] Vol = 283.8 Cell: 7.348 7.358 7.364 119.97 119.27 90.38 Volume: 283.81 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option [ 6] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 254 266 260 0 390 355 345 514 N (int>3sigma) = 0 28 31 47 0 53 73 79 114 Mean intensity = 0.0 1.3 1.2 1.9 0.0 1.5 34.1 41.5 40.6 Mean int/sigma = 0.0 1.5 1.6 2.2 0.0 1.7 4.4 5.1 5.0 Crystal system TETRAGONAL and Lattice type I selected Mean |E*E-1| = 3.792 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41/43 a-- -c- --d N 3 16 50 40 N I>3s 0 0 17 0 0.0 0.0 2.6 0.0 0.6 0.3 3.0 0.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) I4(1)/amd 1 1 141 C N N N N 41 526 0.196 307 I4(1)/amd 4/mmm Tetragonal (1) x, y, z (2) -x+1/2,-y, z+1/2 (3) -y+1/4, x+3/4, z+1/4 (4) y+1/4,-x+1/4, z+3/4 (5) -x+1/2, y,-z+1/2 (6) x,-y,-z (7) y+1/4, x+3/4,-z+1/4 (8) -y+1/4,-x+1/4,-z+3/4 (9) -x,-y,-z (10) x+1/2, y,-z+1/2 (11) y+3/4,-x+1/4,-z+3/4 (12) -y+3/4, x+3/4,-z+1/4 (13) x+1/2,-y, z+1/2 (14) -x, y, z (15) -y+3/4,-x+1/4, z+3/4 (16) y+3/4, x+3/4, z+1/4 Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in I4(1)/amd REM I4(1)/amd (#141 in standard setting) CELL 0.71073 7.364230 7.437053 10.364360 89.9145 89.7982 89.6352 ZERR 1.00 0.021913 0.006276 0.014130 0.0010 0.0010 0.1483 LATT 2 SYMM -x+1/2,-y, z+1/2 SYMM -y+1/4, x+3/4, z+1/4 SYMM y+1/4,-x+1/4, z+3/4 SYMM -x+1/2, y,-z+1/2 SYMM x,-y,-z SYMM y+1/4, x+3/4,-z+1/4 SYMM -y+1/4,-x+1/4,-z+3/4 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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: P4/m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 868646- 120113 94 87 62 1.4 306545.38 24.61 0.165 0.165 112093- 3431 111 102 62 1.6 21794.82 5.10 0.213 0.195 3415- 1576 121 114 62 1.8 1988.63 1.83 0.529 0.540 1566- 1062 104 100 62 1.6 1237.35 1.35 0.543 0.571 1061- 733 97 95 62 1.5 861.66 1.10 0.533 0.540 733- 480 93 88 62 1.4 549.66 0.87 0.402 0.410 473- 277 89 88 62 1.4 370.02 0.75 0.622 0.700 276- 136 97 97 62 1.6 216.87 0.61 0.688 0.753 136- -18 98 98 62 1.6 55.52 0.25 0.904 2.618 -18- -545 82 81 67 1.2 -157.56 -0.28 0.949 2.427 ------------------------------------------------------------------------------------------- 868646- -545 986 950 625 1.5 30967.86 3.49 0.174 0.173 Statistics vs resolution - point group symmetry: P4/m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.43 173 155 62 2.5 64658.43 7.36 0.155 0.153 0.028 1.43-1.12 133 119 62 1.9 43328.37 4.43 0.103 0.102 0.052 1.12-0.97 112 110 62 1.8 27246.20 3.05 0.222 0.220 0.073 0.97-0.87 100 98 62 1.6 36119.73 3.71 0.232 0.232 0.069 0.87-0.80 89 89 63 1.4 19741.10 2.32 0.059 0.059 0.101 0.80-0.75 81 81 62 1.3 18392.32 2.14 0.366 0.366 0.107 0.75-0.70 79 79 62 1.3 21692.87 2.36 0.396 0.396 0.095 0.70-0.65 75 75 63 1.2 15283.41 1.96 0.107 0.107 0.129 0.65-0.60 70 70 62 1.1 12290.30 1.65 0.793 0.887 0.140 0.60-0.49 74 74 65 1.1 9965.75 1.57 0.074 0.075 0.162 ------------------------------------------------------------------------------------------------------ inf-0.49 986 950 625 1.5 30967.86 3.49 0.174 0.173 0.065 inf-0.65 842 806 498 1.6 34518.21 3.82 0.176 0.175 0.060 Statistics vs resolution (taking redundancy into account) - point group symmetry: P4/m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.43 155 63 62 98.4 2.5 64658.43 10.55 0.155 0.018 1.43-1.12 119 62 62 100.0 1.9 43328.37 5.80 0.103 0.036 1.12-0.97 110 63 62 98.4 1.8 27246.20 3.88 0.222 0.064 0.97-0.87 98 64 62 96.9 1.6 36119.73 4.68 0.232 0.048 0.87-0.80 89 69 63 91.3 1.4 19741.10 2.71 0.059 0.094 0.80-0.75 81 77 62 80.5 1.3 18392.32 2.60 0.366 0.075 0.75-0.70 79 77 62 80.5 1.3 21692.87 2.78 0.396 0.067 0.70-0.65 75 114 63 55.3 1.2 15283.41 2.21 0.107 0.087 0.65-0.60 70 153 62 40.5 1.1 12290.30 1.75 0.793 0.883 0.60-0.49 74 626 65 10.4 1.1 9965.75 1.83 0.074 0.094 -------------------------------------------------------------------------------------------- inf-0.49 950 1373 625 45.5 1.5 30967.86 4.53 0.174 0.039 inf-0.65 806 589 498 84.6 1.6 34518.21 5.02 0.176 0.037 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 -1.0 -1.0 0.0 0.0 1.0 -1.0 1.0 0.0 RRPPROF to HKL transformation matrix: -1.0 -1.0 -1.0 0.0 0.0 1.0 -1.0 1.0 0.0 No constraint UB - matrix: -0.020660 -0.002856 -0.066750 ( 0.000053 0.000071 0.000038 ) -0.078662 -0.051575 0.013672 ( 0.000049 0.000065 0.000035 ) -0.051686 0.080189 0.006144 ( 0.000057 0.000075 0.000040 ) M - matrix: 0.009286 -0.000029 -0.000014 ( 0.000010 0.000008 0.000005 ) -0.000029 0.009098 -0.000022 ( 0.000008 0.000014 0.000006 ) -0.000014 -0.000022 0.004680 ( 0.000005 0.000006 0.000005 ) Constraint UB - matrix: -0.020660 -0.002856 -0.066750 ( 0.000053 0.000071 0.000038 ) -0.078662 -0.051575 0.013672 ( 0.000049 0.000065 0.000035 ) -0.051686 0.080189 0.006144 ( 0.000057 0.000075 0.000040 ) M - matrix: 0.009278 0.000000 0.000000 ( 0.000005 0.000000 0.000000 ) 0.000000 0.009278 0.000000 ( 0.000000 0.000005 0.000000 ) 0.000000 0.000000 0.004652 ( 0.000000 0.000000 0.000003 ) unit cell: 7.361(4) 7.436(5) 10.368(6) 89.81(5) 89.88(5) 89.82(5) V = 567.5(6) unit cell: 7.3794(19) 7.3794(19) 10.421(3) 90.0 90.0 90.0 V = 567.5(3) Laue class changed... Laue class: 4/mmm - Friedel mate is equivalent Point group: 4/mmm Lattice type: I-lattice (extinction condition applied) Run 1 Omega scan: (-97.000 - 3.000,100 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-631.0000 max=6112769.0000 PROFFIT INFO: signal sum lp corr: min=-491.5011 max=766620.7055 PROFFIT INFO: background sum: min=224.0000 max=5938.0000 PROFFIT INFO: background sum sig2: min=503.0000 max=4982.0000 PROFFIT INFO: num of signal pixels: min=50 max=497 PROFFIT INFO: Inet: min=-786.4017 max=1226593.1250 PROFFIT INFO: sig(Inet): min=63.5019 max=17638.9316 PROFFIT INFO: Inet/sig(Inet): min=-1.71 max=193.53 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 240 768 1122 1290 1374 1582 1682 1764 1890 1962 1972 Percent 12.2 38.9 56.9 65.4 69.7 80.2 85.3 89.5 95.8 99.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 986 100.00 (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 986 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1226593- 108045 98 309341.85 68.28 100.00 107613- 3163 98 20724.69 16.99 100.00 3151- 1748 98 2415.71 5.88 92.86 1738- 1054 98 1346.40 3.40 37.76 1051- 720 98 867.52 1.92 10.20 717- 454 98 577.18 1.43 5.10 454- 271 98 349.95 1.01 2.04 270- 88 98 170.97 0.48 0.00 87- -28 98 34.56 0.13 0.00 -28- -786 104 -201.15 -0.38 0.00 ------------------------------------------------------------------------------------ 1226593- -786 986 33357.31 9.85 34.58 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.65 98 71010.44 12.77 66.33 1.65- 1.23 98 48664.92 16.45 52.04 1.23- 1.05 98 65916.26 19.73 66.33 1.05- 0.95 98 28926.58 9.42 21.43 0.95- 0.87 98 45273.11 13.90 51.02 0.87- 0.80 98 16068.26 5.82 22.45 0.80- 0.75 98 14703.96 5.07 20.41 0.75- 0.71 98 21059.29 7.08 15.31 0.71- 0.67 98 21111.02 7.25 26.53 0.67- 0.63 104 2715.26 1.53 5.77 ------------------------------------------------------------------------------------ 6.01- 0.63 986 33357.31 9.85 34.58 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:20:00 2019 Sorting 986 observations 59 unique observations with > 7.00 F2/sig(F2) 986 observations in 1 runs Run # start # end # total # 1 0 99 100 Total number of frames 100 Maximum number of 59 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 986 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 49 50 Total number of frames 50 Frame #25 of 50 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: 3.1 (Out of 216 removed 30 = 186, unique = 60) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m2/m2/m 186 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 Frame #25 of 50 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 60 unique data precomputed (should be 60) 60 unique data with 186 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.1 (Out of 186 removed 0 = 186, unique = 60) 60 unique data precomputed (should be 60) 60 unique data with 186 observations RMS deviation of equivalent data = 0.23799 Rint = 0.12017 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.10530, wR= 0.22879 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15186, wR= 0.21029, Acormin=0.203, Acormax=1.236, Acor_av=0.457 F test: Probability=0.000, F= 0.462 Trying model 2 (ne=2, no=1)... Results: Rint= 0.15560, wR= 0.20763, Acormin=0.167, Acormax=0.922, Acor_av=0.460 F test: Probability=0.000, F= 0.429 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10056, wR= 0.13754, Acormin=0.112, Acormax=0.943, Acor_av=0.411 F test: Probability=0.000, F= 0.974 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09892, wR= 0.13453, Acormin=0.066, Acormax=0.972, Acor_av=0.427 F test: Probability=0.000, F= 0.979 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08126, wR= 0.10431, Acormin=0.054, Acormax=0.955, Acor_av=0.447 F test: Probability=0.944, F= 1.357 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: 0.12335 There are 49 active scales (one needs to be fixed) Refinement control: frame scale #11 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 53 pars with 1431 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.23799 Using Levenberg-Marquardt: 0.00010 New wR= 0.15322 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.12017 with corrections 0.13093 Rint for all data: 0.12335 with corrections 0.13455 0 observations identified as outliers and rejected Cycle 2 wR= 0.15322 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= 0.14879 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.12017 with corrections 0.11669 Rint for all data: 0.12335 with corrections 0.12023 0 observations identified as outliers and rejected Cycle 3 wR= 0.14879 Using Levenberg-Marquardt: 0.10000 New wR= 0.16080 Using Levenberg-Marquardt: 1.00000 New wR= 0.14989 Using Levenberg-Marquardt: 10.00000 New wR= 0.14900 Using Levenberg-Marquardt: 100.00000 New wR= 0.14881 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.12017 with corrections 0.11669 Rint for all data: 0.12335 with corrections 0.12023 Final wR= 0.14881 Final frame scales: Min= 0.3295 Max= 1.2318 Final absorption correction factors: Amin= 0.3928 Amax= 1.2819 PROFFIT INFO: Inet (after scale3 abspack): min=-938.7335 max=1084379.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=46.5422 max=22256.7031 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 6, Friedel: 1 Min/max for: run:1/1 frame:1/100 986 reflections read from tmp file 139 reflections are rejected (65 as outliers, 74 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8+ Number of groups: 0 102 86 64 13 7 2 1 Initial Chi^2= 0.83695 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.96612 Current error model SIG(F2)^2 = 144.74*I_RAW + 0.00*I_BACK+(0.05233*)^2 Cycle 2, Chi^2= 1.00102 Current error model SIG(F2)^2 = 144.36*I_RAW + 0.00*I_BACK+(0.03765*)^2 Cycle 3, Chi^2= 1.00026 Current error model SIG(F2)^2 = 146.43*I_RAW + 0.00*I_BACK+(0.03229*)^2 Cycle 4, Chi^2= 1.00022 Current error model SIG(F2)^2 = 147.41*I_RAW + 0.00*I_BACK+(0.02974*)^2 Cycle 5, Chi^2= 1.00013 Current error model SIG(F2)^2 = 147.90*I_RAW + 0.00*I_BACK+(0.02852*)^2 Cycle 6, Chi^2= 1.00007 Current error model SIG(F2)^2 = 148.13*I_RAW + 0.00*I_BACK+(0.02794*)^2 Cycle 7, Chi^2= 1.00003 Current error model SIG(F2)^2 = 148.24*I_RAW + 0.00*I_BACK+(0.02767*)^2 Cycle 8, Chi^2= 1.00002 Current error model SIG(F2)^2 = 148.30*I_RAW + 0.00*I_BACK+(0.02755*)^2 Final Chi^2= 1.00002 Final error model SIG(F2)^2 = 148.30*I_RAW + 0.00*I_BACK+(0.02755*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1084380- 88061 98 317726.00 25.26 100.00 87049- 3792 98 18657.05 9.50 100.00 3749- 1764 98 2485.94 3.96 81.63 1753- 1012 98 1342.25 2.88 29.59 1001- 650 98 814.16 2.01 5.10 648- 408 98 515.54 1.69 2.04 403- 240 98 318.11 1.54 2.04 239- 90 98 157.14 1.18 5.10 83- -23 98 32.71 0.42 1.02 -25- -939 104 -199.54 -0.78 0.00 ------------------------------------------------------------------------------------ 1084380- -939 986 33975.70 4.73 32.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.65 98 70699.58 7.69 65.31 1.65- 1.23 98 54657.38 6.37 47.96 1.23- 1.05 98 72662.85 7.47 64.29 1.05- 0.95 98 29292.87 4.10 20.41 0.95- 0.87 98 45434.07 6.62 45.92 0.87- 0.80 98 13740.72 3.14 21.43 0.80- 0.75 98 13939.40 2.98 14.29 0.75- 0.71 98 19279.74 3.96 16.33 0.71- 0.67 98 19309.61 3.87 24.49 0.67- 0.63 104 2658.18 1.32 5.77 ------------------------------------------------------------------------------------ 6.01- 0.63 986 33975.70 4.73 32.45 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.65 98 70699.58 7.69 65.31 6.01- 1.23 196 62678.48 7.03 56.63 6.01- 1.05 294 66006.60 7.18 59.18 6.01- 0.95 392 56828.17 6.41 49.49 6.01- 0.87 490 54549.35 6.45 48.78 6.01- 0.80 588 47747.91 5.90 44.22 6.01- 0.75 686 42918.12 5.48 39.94 6.01- 0.71 784 39963.33 5.29 36.99 6.01- 0.67 882 37668.47 5.14 35.60 6.01- 0.63 986 33975.70 4.73 32.45 ------------------------------------------------------------------------------------ 6.01- 0.63 986 33975.70 4.73 32.45 Scale applied to data: s=0.922185 (maximum obs:1084379.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.120; Rsigma 0.046: data 986 -> merged 358 With outlier rejection... Rint 0.086; Rsigma 0.047: data 949 -> merged 358 Rejected total: 37, method kkm 37, method Blessing 0 Completeness direct cell (a, b, c) = (7.379, 7.379, 10.421), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627353, 6.022412 completeness table (Laue group: I4/mmm (tetra-c), Friedel couples are equivalent) range data theory redun '%' total 7.42 - 1.59 33 34 3.09 97.06 102 1.59 - 1.20 33 34 2.97 97.06 98 1.20 - 1.02 34 34 2.88 100.00 98 1.02 - 0.91 34 34 3.15 100.00 107 0.91 - 0.85 34 34 2.68 100.00 91 0.85 - 0.80 34 34 2.79 100.00 95 0.80 - 0.75 33 34 2.48 97.06 82 0.75 - 0.72 31 34 2.55 91.18 79 0.72 - 0.68 31 34 2.45 91.18 76 0.68 - 0.65 37 41 2.27 90.24 84 --------------------------------------------------------------- 7.42 - 0.65 334 347 2.73 96.25 912 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:19:59 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.389630 7.363616 7.437053 120.4722 120.4926 89.2579 950 Reflections read from file xs2212a.hkl 514 Reflections used for space-group determination (up to diffraction limit of 0.82A); mean (I/sigma) = 4.97 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 251 265 260 254 388 343 353 514 N (int>3sigma) = 0 28 27 47 28 51 78 77 114 Mean intensity = 0.0 1.2 1.3 1.9 1.3 1.5 42.7 41.1 40.6 Mean int/sigma = 0.0 1.5 1.5 2.2 1.5 1.8 5.1 5.2 5.0 Lattice type: P chosen Volume: 283.81 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.348 7.358 7.364 119.97 119.27 90.38 Niggli form: a.a = 53.989 b.b = 54.143 c.c = 54.223 b.c = -27.067 a.c = -26.451 a.b = -0.356 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 6] err= 0.524 TETRAGONAL I-lattice R(int) = 0.140 [ 244] Vol = 567.6 Cell: 7.364 7.437 10.364 89.91 89.80 89.64 Volume: 567.62 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.672 TETRAGONAL I-lattice R(int) = 0.189 [ 249] Vol = 567.6 Cell: 7.348 7.358 10.499 90.26 89.46 90.38 Volume: 567.62 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.584 TETRAGONAL I-lattice R(int) = 0.140 [ 244] Vol = 567.6 Cell: 7.437 7.364 10.364 90.20 89.91 90.36 Volume: 567.62 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.734 ORTHORHOMBIC F-lattice R(int) = 0.159 [ 228] Vol = 1135.2 Cell: 10.364 10.433 10.499 89.44 90.20 89.92 Volume: 1135.24 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.404 ORTHORHOMBIC I-lattice R(int) = 0.152 [ 258] Vol = 567.6 Cell: 10.364 7.437 7.364 89.64 89.80 89.91 Volume: 567.62 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.650 ORTHORHOMBIC I-lattice R(int) = 0.169 [ 272] Vol = 567.6 Cell: 7.348 7.358 10.499 89.74 90.54 90.38 Volume: 567.62 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.280 MONOCLINIC I-lattice R(int) = 0.078 [ 120] Vol = 567.6 Cell: 7.364 10.364 7.437 89.91 90.36 90.20 Volume: 567.62 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.599 MONOCLINIC I-lattice R(int) = 0.173 [ 126] Vol = 567.6 Cell: 7.364 10.433 7.390 90.34 90.74 89.54 Volume: 567.62 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.221 MONOCLINIC I-lattice R(int) = 0.078 [ 120] Vol = 567.6 Cell: 7.437 10.364 7.364 90.20 90.36 89.91 Volume: 567.62 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.356 MONOCLINIC I-lattice R(int) = 0.161 [ 211] Vol = 567.6 Cell: 7.348 7.358 10.499 90.26 90.54 89.62 Volume: 567.62 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.405 MONOCLINIC I-lattice R(int) = 0.196 [ 118] Vol = 567.6 Cell: 7.348 10.499 7.358 90.26 90.38 89.46 Volume: 567.62 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.750 MONOCLINIC I-lattice R(int) = 0.196 [ 118] Vol = 567.6 Cell: 7.348 10.499 7.358 89.74 90.38 90.54 Volume: 567.62 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.137 [ 29] Vol = 283.8 Cell: 7.348 7.358 7.364 119.97 119.27 90.38 Volume: 283.81 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option [ 6] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 254 266 260 0 390 355 345 514 N (int>3sigma) = 0 28 31 47 0 53 73 79 114 Mean intensity = 0.0 1.3 1.2 1.9 0.0 1.5 34.1 41.5 40.6 Mean int/sigma = 0.0 1.5 1.6 2.2 0.0 1.7 4.4 5.1 5.0 Crystal system TETRAGONAL and Lattice type I selected Mean |E*E-1| = 3.792 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41/43 a-- -c- --d N 3 16 50 40 N I>3s 0 0 17 0 0.0 0.0 2.6 0.0 0.6 0.3 3.0 0.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) I4(1)/amd 1 1 141 C N N N N 41 526 0.196 307 I4(1)/amd 4/mmm Tetragonal (1) x, y, z (2) -x+1/2,-y, z+1/2 (3) -y+1/4, x+3/4, z+1/4 (4) y+1/4,-x+1/4, z+3/4 (5) -x+1/2, y,-z+1/2 (6) x,-y,-z (7) y+1/4, x+3/4,-z+1/4 (8) -y+1/4,-x+1/4,-z+3/4 (9) -x,-y,-z (10) x+1/2, y,-z+1/2 (11) y+3/4,-x+1/4,-z+3/4 (12) -y+3/4, x+3/4,-z+1/4 (13) x+1/2,-y, z+1/2 (14) -x, y, z (15) -y+3/4,-x+1/4, z+3/4 (16) y+3/4, x+3/4, z+1/4 Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in I4(1)/amd REM I4(1)/amd (#141 in standard setting) CELL 0.71073 7.364230 7.437053 10.364360 89.9145 89.7982 89.6352 ZERR 1.00 0.021913 0.006276 0.014130 0.0010 0.0010 0.1483 LATT 2 SYMM -x+1/2,-y, z+1/2 SYMM -y+1/4, x+3/4, z+1/4 SYMM y+1/4,-x+1/4, z+3/4 SYMM -x+1/2, y,-z+1/2 SYMM x,-y,-z SYMM y+1/4, x+3/4,-z+1/4 SYMM -y+1/4,-x+1/4,-z+3/4 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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: I4/mmm # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 1051100- 146884 78 68 35 1.9 369499.62 26.96 0.080 0.090 133307- 4707 101 92 35 2.6 37178.57 11.85 0.091 0.091 4056- 1959 102 96 35 2.7 2765.96 4.22 0.153 0.160 1860- 1065 104 101 35 2.9 1419.29 2.95 0.178 0.192 1061- 621 102 102 35 2.9 791.87 1.87 0.265 0.291 619- 403 100 99 35 2.8 509.36 1.66 0.395 0.447 403- 262 108 107 35 3.1 323.23 1.40 0.417 0.441 262- 99 97 93 35 2.7 165.80 0.96 0.572 0.715 96- -1 102 101 35 2.9 47.61 0.54 0.867 2.327 -4- -784 92 90 43 2.1 -146.45 -0.49 0.704 0.875 ------------------------------------------------------------------------------------------- 1051100- -784 986 949 358 2.7 30693.48 4.46 0.086 0.094 Statistics vs resolution - point group symmetry: I4/mmm resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.57 113 108 35 3.1 78975.60 8.47 0.104 0.116 0.031 1.51-1.17 110 103 35 2.9 54557.68 5.71 0.069 0.071 0.039 1.17-1.01 109 107 35 3.1 23707.86 4.01 0.040 0.037 0.046 1.01-0.91 109 107 35 3.1 30096.05 4.73 0.055 0.063 0.045 0.91-0.84 96 91 35 2.6 38750.18 5.92 0.027 0.030 0.052 0.84-0.78 98 95 36 2.6 19204.20 3.78 0.256 0.257 0.061 0.78-0.73 93 91 35 2.6 2109.34 1.35 0.397 0.425 0.201 0.73-0.70 91 89 35 2.5 20382.88 3.97 0.089 0.092 0.068 0.70-0.67 85 80 36 2.2 19954.73 3.81 0.083 0.081 0.077 0.66-0.63 82 78 41 1.9 3451.54 1.45 0.262 0.266 0.171 ------------------------------------------------------------------------------------------------------ inf-0.63 986 949 358 2.7 30693.48 4.46 0.086 0.094 0.047 inf-0.66 945 910 333 2.7 31736.47 4.57 0.085 0.093 0.046 Statistics vs resolution (taking redundancy into account) - point group symmetry: I4/mmm resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.57 108 36 35 97.2 3.1 78975.60 14.85 0.104 0.020 1.51-1.17 103 36 35 97.2 2.9 54557.68 9.32 0.069 0.025 1.17-1.01 107 35 35 100.0 3.1 23707.86 6.69 0.040 0.028 1.01-0.91 107 35 35 100.0 3.1 30096.05 8.11 0.055 0.027 0.91-0.84 91 35 35 100.0 2.6 38750.18 9.73 0.027 0.033 0.84-0.78 95 36 36 100.0 2.6 19204.20 5.75 0.256 0.041 0.78-0.73 91 38 35 92.1 2.6 2109.34 2.14 0.397 0.405 0.73-0.70 89 36 35 97.2 2.5 20382.88 6.19 0.089 0.043 0.70-0.67 80 40 36 90.0 2.2 19954.73 5.88 0.083 0.049 0.66-0.63 78 66 41 62.1 1.9 3451.54 1.83 0.262 0.133 -------------------------------------------------------------------------------------------- inf-0.63 949 393 358 91.1 2.7 30693.48 7.31 0.086 0.030 inf-0.66 910 344 333 96.8 2.7 31736.47 7.53 0.085 0.030 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:21:08 2019) ID: 3668; threads 40; handles 810; mem 514288.00 (1204700.00)kB; time: 1w 4d 22h 31m 56s MEMORY INFO: Memory PF:70.0, Ph:525.0, V:1176.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:502.2,peak PF: 700.2, WS: 470.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:72.0, Ph:527.0, V:1178.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:504.0,peak PF: 700.2, WS: 472.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:21:08 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000095 0.000058 0.000092 ) 0.065981 0.091690 0.025911 ( 0.000085 0.000052 0.000082 ) 0.044418 0.058869 0.132122 ( 0.000103 0.000063 0.000100 ) 7.34808 ( 0.00624 ) 7.34732 ( 0.00605 ) 7.36303 ( 0.00649 ) 119.94370 ( 0.08943 ) 119.84600 ( 0.09040 ) 90.15964 ( 0.06779 ) V = 281.59 Selected cell (from UM rr/UM ttt/UM f): 44 7.3481 7.3473 7.3630 119.9437 119.8460 90.1596 aP Cross checking gral lattice... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:21:08 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087271 -0.045830 0.019137 ( 0.000095 0.000058 0.000092 ) 0.065981 0.091690 0.025911 ( 0.000085 0.000052 0.000082 ) 0.044418 0.058869 0.132122 ( 0.000103 0.000063 0.000100 ) M - matrix: 0.013924 0.004590 0.009322 ( 0.000022 0.000013 0.000018 ) 0.004590 0.014009 0.009355 ( 0.000013 0.000013 0.000014 ) 0.009322 0.009355 0.018503 ( 0.000018 0.000014 0.000027 ) unit cell: 7.348(6) 7.347(6) 7.363(6) 119.94(9) 119.85(9) 90.16(7) V = 281.6(4) Lattice type P used *** 3D peak analysis started - run 1 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb PROFFITPEAK info: 384 peaks in the peak location table UB fit with 149 obs out of 232 (total:232,skipped:0) (64.22%) UB - matrix: 0.087053 -0.045748 0.018695 ( 0.000091 0.000054 0.000110 ) 0.065636 0.092116 0.026769 ( 0.000094 0.000056 0.000114 ) 0.044281 0.058458 0.132317 ( 0.000118 0.000070 0.000143 ) M - matrix: 0.013847 0.004652 0.009244 ( 0.000023 0.000014 0.000021 ) 0.004652 0.013996 0.009346 ( 0.000014 0.000014 0.000017 ) 0.009244 0.009346 0.018574 ( 0.000021 0.000017 0.000039 ) unit cell: 7.376(7) 7.358(7) 7.366(9) 120.17(11) 119.89(11) 90.01(7) V = 282.5(5) UB fit with 149 obs out of 232 (total:232,skipped:0) (64.22%) UB - matrix: 0.087053 -0.045748 0.018695 ( 0.000091 0.000054 0.000110 ) 0.065636 0.092116 0.026769 ( 0.000094 0.000056 0.000114 ) 0.044281 0.058458 0.132317 ( 0.000118 0.000070 0.000143 ) M - matrix: 0.013847 0.004652 0.009244 ( 0.000023 0.000014 0.000021 ) 0.004652 0.013996 0.009346 ( 0.000014 0.000014 0.000017 ) 0.009244 0.009346 0.018574 ( 0.000021 0.000017 0.000039 ) unit cell: 7.376(7) 7.358(7) 7.366(9) 120.17(11) 119.89(11) 90.01(7) V = 282.5(5) OTKP changes: 80 1 1 1 OTKP changes: 80 1 1 1 OTKP changes: 80 1 1 1 UB - matrix: 0.087121 -0.045926 0.017970 ( 0.000092 0.000057 0.000102 ) 0.065035 0.092304 0.027245 ( 0.000105 0.000065 0.000116 ) 0.045328 0.057881 0.131838 ( 0.000109 0.000068 0.000121 ) M - matrix: 0.013874 0.004625 0.009313 ( 0.000023 0.000014 0.000020 ) 0.004625 0.013979 0.009320 ( 0.000014 0.000015 0.000016 ) 0.009313 0.009320 0.018447 ( 0.000020 0.000016 0.000033 ) UB fit with 187 obs out of 232 (total:232,skipped:0) (80.60%) unit cell: 7.406(7) 7.367(7) 7.440(8) 120.31(11) 120.46(11) 89.50(8) V = 285.0(5) UB fit with 187 obs out of 232 (total:232,skipped:0) (80.60%) UB - matrix: 0.087147 -0.045946 0.017901 ( 0.000093 0.000058 0.000102 ) 0.065031 0.092305 0.027243 ( 0.000103 0.000064 0.000112 ) 0.045430 0.057865 0.131834 ( 0.000108 0.000067 0.000118 ) M - matrix: 0.013887 0.004627 0.009321 ( 0.000023 0.000014 0.000019 ) 0.004627 0.013980 0.009321 ( 0.000014 0.000015 0.000016 ) 0.009321 0.009321 0.018443 ( 0.000019 0.000016 0.000032 ) unit cell: 7.405(7) 7.368(7) 7.443(8) 120.32(11) 120.48(10) 89.48(8) V = 284.9(5) OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 UB - matrix: 0.087281 -0.046000 0.017745 ( 0.000094 0.000063 0.000107 ) 0.064890 0.092335 0.027276 ( 0.000093 0.000062 0.000105 ) 0.045572 0.057837 0.131880 ( 0.000101 0.000067 0.000114 ) M - matrix: 0.013905 0.004612 0.009329 ( 0.000022 0.000014 0.000019 ) 0.004612 0.013987 0.009330 ( 0.000014 0.000015 0.000016 ) 0.009329 0.009330 0.018451 ( 0.000019 0.000016 0.000031 ) UB fit with 196 obs out of 232 (total:232,skipped:0) (84.48%) unit cell: 7.400(7) 7.368(7) 7.447(8) 120.39(10) 120.53(10) 89.35(7) V = 284.7(5) 232 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1319 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087281 -0.046000 0.017745 ( 0.000094 0.000063 0.000107 ) 0.064890 0.092335 0.027276 ( 0.000093 0.000062 0.000105 ) 0.045572 0.057837 0.131880 ( 0.000101 0.000067 0.000114 ) M - matrix: 0.013905 0.004612 0.009329 ( 0.000022 0.000014 0.000019 ) 0.004612 0.013987 0.009330 ( 0.000014 0.000015 0.000016 ) 0.009329 0.009330 0.018451 ( 0.000019 0.000016 0.000031 ) UB fit with 196 obs out of 232 (total:232,skipped:0) (84.48%) unit cell: 7.400(7) 7.368(7) 7.447(8) 120.39(10) 120.53(10) 89.35(7) V = 284.7(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 206 obs out of 232 (total:232,skipped:0) (88.79%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 219 peaks identified as outliers and rejected 219 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 219 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 219 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.995 ( 0.536) | 0.878 ( 0.220) | 1.577 ( 2.146) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.76- 1.57 | 22 | 0.856 ( 0.093) | 0.889 ( 0.144) | 0.713 ( 0.349) | 1.57- 1.35 | 22 | 0.930 ( 0.066) | 0.994 ( 0.119) | 0.998 ( 0.456) | 1.35- 1.16 | 22 | 0.948 ( 0.076) | 1.031 ( 0.130) | 1.009 ( 0.694) | 1.16- 1.00 | 22 | 0.927 ( 0.094) | 0.960 ( 0.175) | 0.881 ( 0.280) | 1.00- 0.88 | 22 | 0.959 ( 0.073) | 0.984 ( 0.111) | 1.217 ( 0.529) | 0.88- 0.78 | 22 | 0.983 ( 0.056) | 1.031 ( 0.143) | 1.120 ( 0.322) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.945 ( 0.105) | 1.345 ( 0.508) | 0.69- 0.63 | 21 | 0.941 ( 0.037) | 0.919 ( 0.102) | 1.271 ( 0.457) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 219 | 0.935 ( 0.190) | 0.946 ( 0.157) | 1.090 ( 0.848) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 200 obs out of 219 (total:219,skipped:0) (91.32%) UB - matrix: 0.087419 -0.046160 0.017666 ( 0.000089 0.000056 0.000089 ) 0.064828 0.092239 0.027413 ( 0.000081 0.000051 0.000081 ) 0.045477 0.057583 0.131788 ( 0.000100 0.000063 0.000100 ) M - matrix: 0.013913 0.004563 0.009315 ( 0.000021 0.000012 0.000017 ) 0.004563 0.013955 0.009302 ( 0.000012 0.000013 0.000013 ) 0.009315 0.009302 0.018432 ( 0.000017 0.000013 0.000027 ) unit cell: 7.394(6) 7.372(6) 7.451(7) 120.45(9) 120.59(9) 89.15(7) V = 284.7(4) OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 UB - matrix: 0.087503 -0.046060 0.017517 ( 0.000092 0.000059 0.000091 ) 0.064714 0.092375 0.027238 ( 0.000084 0.000054 0.000084 ) 0.045643 0.057892 0.132051 ( 0.000097 0.000062 0.000096 ) M - matrix: 0.013928 0.004590 0.009323 ( 0.000021 0.000013 0.000017 ) 0.004590 0.014006 0.009354 ( 0.000013 0.000013 0.000013 ) 0.009323 0.009354 0.018486 ( 0.000017 0.000013 0.000026 ) UB fit with 206 obs out of 219 (total:219,skipped:0) (94.06%) unit cell: 7.385(6) 7.366(6) 7.441(6) 120.52(9) 120.49(9) 89.21(7) V = 283.8(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1316 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087503 -0.046060 0.017517 ( 0.000092 0.000059 0.000091 ) 0.064714 0.092375 0.027238 ( 0.000084 0.000054 0.000084 ) 0.045643 0.057892 0.132051 ( 0.000097 0.000062 0.000096 ) M - matrix: 0.013928 0.004590 0.009323 ( 0.000021 0.000013 0.000017 ) 0.004590 0.014006 0.009354 ( 0.000013 0.000013 0.000013 ) 0.009323 0.009354 0.018486 ( 0.000017 0.000013 0.000026 ) UB fit with 206 obs out of 219 (total:219,skipped:0) (94.06%) unit cell: 7.385(6) 7.366(6) 7.441(6) 120.52(9) 120.49(9) 89.21(7) V = 283.8(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 211 obs out of 219 (total:219,skipped:0) (96.35%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 214 peaks identified as outliers and rejected 214 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 214 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 214 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.995 ( 0.545) | 0.843 ( 0.183) | 1.635 ( 2.377) | 2.60- 1.75 | 21 | 0.822 ( 0.086) | 0.812 ( 0.150) | 0.735 ( 0.315) | 1.75- 1.57 | 21 | 0.859 ( 0.089) | 0.893 ( 0.144) | 0.685 ( 0.239) | 1.56- 1.35 | 21 | 0.938 ( 0.067) | 1.004 ( 0.122) | 1.123 ( 0.524) | 1.35- 1.16 | 21 | 0.953 ( 0.073) | 1.024 ( 0.122) | 0.912 ( 0.397) | 1.16- 1.00 | 21 | 0.941 ( 0.078) | 0.976 ( 0.177) | 0.967 ( 0.399) | 1.00- 0.88 | 21 | 0.968 ( 0.078) | 1.011 ( 0.130) | 1.164 ( 0.510) | 0.88- 0.79 | 21 | 0.978 ( 0.051) | 1.012 ( 0.138) | 1.186 ( 0.362) | 0.79- 0.72 | 21 | 0.984 ( 0.039) | 0.964 ( 0.116) | 1.263 ( 0.463) | 0.72- 0.63 | 25 | 0.950 ( 0.039) | 0.933 ( 0.096) | 1.317 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 214 | 0.939 ( 0.190) | 0.947 ( 0.156) | 1.103 ( 0.887) | 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 | 21 | 0.976 ( 0.043) | 1.060 ( 0.060) | 1.159 ( 0.490) | 12.7-16.5 | 21 | 1.078 ( 0.435) | 1.094 ( 0.118) | 1.515 ( 2.173) | 16.5-20.6 | 21 | 0.941 ( 0.066) | 1.012 ( 0.097) | 1.025 ( 0.535) | 20.6-25.0 | 21 | 0.963 ( 0.060) | 1.023 ( 0.105) | 0.996 ( 0.431) | 25.0-29.0 | 21 | 0.947 ( 0.084) | 1.013 ( 0.130) | 1.046 ( 0.483) | 29.0-32.7 | 21 | 0.909 ( 0.088) | 0.935 ( 0.126) | 0.849 ( 0.410) | 33.1-36.4 | 21 | 0.948 ( 0.297) | 0.879 ( 0.125) | 1.216 ( 1.015) | 36.7-38.6 | 21 | 0.843 ( 0.089) | 0.785 ( 0.112) | 1.092 ( 0.574) | 38.6-41.1 | 21 | 0.908 ( 0.098) | 0.893 ( 0.167) | 1.144 ( 0.459) | 41.2-49.8 | 25 | 0.888 ( 0.108) | 0.805 ( 0.113) | 1.005 ( 0.523) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 214 | 0.939 ( 0.190) | 0.947 ( 0.156) | 1.103 ( 0.887) | Fitted profile normalization line parameters e1 dimension: a=-0.0031 b=1.13 e2 dimension: a=-0.0085 b=1.32 e3 dimension: a=0.0023 b=1.01 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 4854 lp-corr: 3597 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 316425 Maximum peak integral for reflections I/sig<= 10000 - raw: 6305075 lp-corr: 954139 PROFFITPEAK - Finished at Wed Aug 21 12:21:13 2019 PROFFITMAIN - Started at Wed Aug 21 12:21:13 2019 OTKP changes: 161 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 180 1 1 1 OTKP changes: 144 1 1 1 OTKP changes: 160 1 1 1 UB - matrix: 0.087442 -0.046074 0.017604 ( 0.000097 0.000059 0.000091 ) 0.064900 0.092355 0.027314 ( 0.000080 0.000049 0.000076 ) 0.045545 0.057868 0.132140 ( 0.000104 0.000063 0.000098 ) M - matrix: 0.013933 0.004601 0.009330 ( 0.000022 0.000012 0.000017 ) 0.004601 0.014001 0.009358 ( 0.000012 0.000013 0.000013 ) 0.009330 0.009358 0.018517 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 214 (total:214,skipped:0) (92.99%) unit cell: 7.383(6) 7.367(6) 7.431(6) 120.48(9) 120.46(9) 89.29(7) V = 283.5(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 199 obs out of 214 (total:214,skipped:0) (92.99%) UB - matrix: 0.087476 -0.046086 0.017534 ( 0.000099 0.000060 0.000091 ) 0.064839 0.092356 0.027314 ( 0.000085 0.000051 0.000078 ) 0.045527 0.057867 0.132176 ( 0.000106 0.000064 0.000098 ) M - matrix: 0.013929 0.004591 0.009322 ( 0.000023 0.000013 0.000018 ) 0.004591 0.014002 0.009363 ( 0.000013 0.000013 0.000013 ) 0.009322 0.009363 0.018524 ( 0.000018 0.000013 0.000026 ) unit cell: 7.381(6) 7.368(6) 7.429(6) 120.52(9) 120.43(9) 89.25(7) V = 283.4(4) OTKP changes: 200 1 1 1 OTKP changes: 200 1 1 1 OTKP changes: 200 1 1 1 UB - matrix: 0.087431 -0.046049 0.017411 ( 0.000101 0.000062 0.000093 ) 0.064759 0.092363 0.027186 ( 0.000086 0.000053 0.000080 ) 0.045577 0.057920 0.132170 ( 0.000099 0.000060 0.000091 ) M - matrix: 0.013915 0.004595 0.009307 ( 0.000023 0.000013 0.000017 ) 0.004595 0.014006 0.009364 ( 0.000013 0.000013 0.000013 ) 0.009307 0.009364 0.018511 ( 0.000017 0.000013 0.000025 ) UB fit with 202 obs out of 214 (total:214,skipped:0) (94.39%) unit cell: 7.381(7) 7.368(6) 7.428(6) 120.52(9) 120.38(9) 89.30(7) V = 283.5(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087430 -0.046050 0.017411 ( 0.000101 0.000062 0.000093 ) 0.064759 0.092363 0.027185 ( 0.000086 0.000053 0.000080 ) 0.045577 0.057920 0.132170 ( 0.000099 0.000060 0.000091 ) M - matrix: 0.013915 0.004595 0.009307 ( 0.000023 0.000013 0.000017 ) 0.004595 0.014006 0.009364 ( 0.000013 0.000013 0.000013 ) 0.009307 0.009364 0.018511 ( 0.000017 0.000013 0.000025 ) UB fit with 202 obs out of 214 (total:214,skipped:0) (94.39%) unit cell: 7.381(7) 7.368(6) 7.428(6) 120.52(9) 120.38(9) 89.30(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 214 (total:214,skipped:0) (96.73%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118181 0.039132 0.078789 ( 0.000076 0.000047 0.000069 ) 0.000039 0.111639 0.056270 ( 0.000074 0.000045 0.000067 ) 0.000030 -0.000044 0.095670 ( 0.000092 0.000057 0.000084 ) M - matrix: 0.013967 0.004629 0.009316 ( 0.000018 0.000010 0.000014 ) 0.004629 0.013995 0.009361 ( 0.000010 0.000011 0.000011 ) 0.009316 0.009361 0.018527 ( 0.000014 0.000011 0.000021 ) UB fit with 209 obs out of 214 (total:214,skipped:0) (97.66%) unit cell: 7.363(5) 7.369(5) 7.413(8) 120.43(9) 120.24(9) 89.52(5) V = 282.7(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: 0.087467 -0.046083 0.017536 ( 0.000099 0.000060 0.000091 ) 0.064846 0.092375 0.027309 ( 0.000085 0.000052 0.000078 ) 0.045520 0.057904 0.132230 ( 0.000106 0.000064 0.000098 ) M - matrix: 0.013928 0.004595 0.009324 ( 0.000023 0.000013 0.000018 ) 0.004595 0.014010 0.009371 ( 0.000013 0.000013 0.000013 ) 0.009324 0.009371 0.018538 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 214 (total:214,skipped:0) (93.46%) unit cell: 7.380(6) 7.367(6) 7.426(6) 120.52(9) 120.42(9) 89.27(7) V = 283.2(4) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 44 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof 1017 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:21:14 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a Laue class: 4/m - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-558.0000 max=6109867.0000 PROFFIT INFO: signal sum lp corr: min=-578.6852 max=792081.7013 PROFFIT INFO: background sum: min=160.0000 max=5938.0000 PROFFIT INFO: background sum sig2: min=520.0000 max=4997.0000 PROFFIT INFO: num of signal pixels: min=50 max=497 PROFFIT INFO: Inet: min=-925.8964 max=1267330.7500 PROFFIT INFO: sig(Inet): min=63.9097 max=17698.8184 PROFFIT INFO: Inet/sig(Inet): min=-1.69 max=164.82 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 113 390 578 663 711 812 866 902 971 1009 1017 Percent 11.1 38.3 56.8 65.2 69.9 79.8 85.2 88.7 95.5 99.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1017 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 1017 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1267331- 116930 101 314971.59 70.65 100.00 114860- 3412 101 25511.01 18.09 100.00 3380- 1771 101 2474.10 6.07 94.06 1753- 1055 101 1334.30 3.16 37.62 1052- 702 101 853.81 1.92 7.92 701- 470 101 586.91 1.45 8.91 468- 262 101 357.47 1.01 1.98 259- 105 101 176.33 0.51 0.00 105- -8 101 45.55 0.17 0.00 -9- -926 108 -203.76 -0.39 0.00 ------------------------------------------------------------------------------------ 1267331- -926 1017 34371.10 10.19 34.81 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.87- 1.82 101 91952.88 16.90 66.34 1.82- 1.34 101 63598.36 20.82 55.45 1.34- 1.13 101 19351.66 8.51 46.53 1.12- 0.98 101 45793.83 14.54 42.57 0.98- 0.90 101 34789.68 10.89 31.68 0.89- 0.81 101 15044.15 5.20 18.81 0.81- 0.74 101 25316.47 8.33 30.69 0.74- 0.68 101 20973.91 6.95 22.77 0.68- 0.62 101 13986.82 4.86 14.85 0.62- 0.49 108 14294.69 5.23 19.44 ------------------------------------------------------------------------------------ 6.87- 0.49 1017 34371.10 10.19 34.81 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:21:15 2019 Sorting 1017 observations 59 unique observations with > 7.00 F2/sig(F2) 1017 observations in 1 runs Run # start # end # total # 1 0 102 103 Total number of frames 103 Maximum number of 59 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1017 observations in 1 runs Run # start # end # total # 1 0 51 52 Total number of frames 52 223 observations > 7.00 F2/sig(F2) 223 observations in 1 runs Run # start # end # total # 1 0 50 51 Total number of frames 51 Frame #25 of 51 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 223 removed 92 = 131, unique = 55) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m 131 observations in 1 runs Run # start # end # total # 1 0 50 51 Total number of frames 51 Frame #25 of 51 skipped from refinement Frame #32 of 51 skipped from refinement Frame #48 of 51 skipped from refinement 3 frames need to be skipped from refinement, because of missing redundant and/or observable data 55 unique data precomputed (should be 55) 55 unique data with 131 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.4 (Out of 131 removed 0 = 131, unique = 55) 55 unique data precomputed (should be 55) 55 unique data with 131 observations RMS deviation of equivalent data = 0.25983 Rint = 0.22284 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.22284, wR= 0.31216 Trying model 1 (ne=2, no=0)... Results: Rint= 0.19263, wR= 0.25476, Acormin=0.159, Acormax=1.514, Acor_av=0.455 F test: Probability=0.829, F= 1.250 Trying model 2 (ne=2, no=1)... Results: Rint= 0.24330, wR= 0.24709, Acormin=-0.170, Acormax=1.388, Acor_av=0.361 F test: Probability=0.000, F= 0.751 Trying model 3 (ne=4, no=0)... Results: Rint= 0.23832, wR= 0.27569, Acormin=0.047, Acormax=1.568, Acor_av=0.228 F test: Probability=0.000, F= 0.713 Trying model 4 (ne=4, no=1)... Results: Rint= 0.24751, wR= 0.25941, Acormin=-0.144, Acormax=1.406, Acor_av=0.217 F test: Probability=0.000, F= 0.629 Trying model 5 (ne=4, no=3)... Results: Rint= 0.12306, wR= 0.14029, Acormin=-0.002, Acormax=1.287, Acor_av=0.260 F test: Probability=0.999, F= 2.244 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: 0.23485 There are 48 active scales (one needs to be fixed) Refinement control: frame scale #22 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 52 pars with 1378 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25983 Using Levenberg-Marquardt: 0.00010 New wR= 0.14370 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.22284 with corrections 0.13834 Rint for all data: 0.23485 with corrections 0.15319 0 observations identified as outliers and rejected Cycle 2 wR= 0.14370 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= 0.49002 Using Levenberg-Marquardt: 0.01000 New wR= 0.12121 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.22284 with corrections 0.10773 Rint for all data: 0.23485 with corrections 0.12246 0 observations identified as outliers and rejected Cycle 3 wR= 0.12121 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.11170 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.22284 with corrections 0.08893 Rint for all data: 0.23485 with corrections 0.10502 0 observations identified as outliers and rejected Cycle 4 wR= 0.11170 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.28052 Using Levenberg-Marquardt: 0.10000 New wR= 0.11172 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.22284 with corrections 0.08926 Rint for all data: 0.23485 with corrections 0.10490 Final wR= 0.11172 Final frame scales: Min= 0.8036 Max= 2.2216 Final absorption correction factors: Amin= 0.1528 Amax= 1.8070 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=-2358.2119 max=2364142.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=36.2519 max=44860.0430 PROFFIT INFO: 2 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\xs2212a\xs2212a.tmp Laue: 5, Friedel: 1 Min/max for: run:1/1 frame:1/102 1015 reflections read from tmp file 515 reflections are rejected (122 as outliers, 393 as groups of 1 refl) Redundancy: 1 2 3 4 5+ Number of groups: 0 183 24 13 2 Initial Chi^2= 3.20862 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.78410 Current error model SIG(F2)^2 = 610.01*I_RAW + 0.00*I_BACK+(0.01426*)^2 Negative value encountered! Resetting parameters to initial values... Cycle 2, Chi^2= 0.99666 Current error model SIG(F2)^2 = 483.44*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 3, Chi^2= 1.00000 Current error model SIG(F2)^2 = 481.82*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 481.82*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2364143- 97365 101 326219.63 25.69 100.00 96377- 3774 101 21455.03 5.66 74.26 3734- 1619 101 2350.87 2.38 12.87 1618- 978 101 1266.00 1.67 7.92 971- 617 101 794.45 1.17 0.99 616- 421 101 513.16 1.04 0.00 416- 222 101 314.53 0.83 0.99 219- 93 101 157.99 0.71 0.99 92- -6 101 40.94 0.30 0.00 -6- -2358 106 -242.96 -0.44 0.00 ------------------------------------------------------------------------------------ 2364143- -2358 1015 35111.94 3.88 19.70 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.87- 1.82 101 96094.18 10.33 43.56 1.82- 1.34 101 75786.26 6.61 35.64 1.34- 1.13 101 23641.97 2.93 21.78 1.12- 0.98 101 47490.48 4.72 17.82 0.98- 0.90 101 34633.88 3.66 17.82 0.89- 0.81 101 15262.01 1.90 7.92 0.81- 0.74 101 19615.26 2.80 14.85 0.74- 0.68 101 17483.72 2.41 12.87 0.68- 0.62 101 11484.70 1.70 10.89 0.62- 0.49 106 10829.07 1.83 14.15 ------------------------------------------------------------------------------------ 6.87- 0.49 1015 35111.94 3.88 19.70 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.87- 1.82 101 96094.18 10.33 43.56 6.87- 1.34 202 85940.22 8.47 39.60 6.87- 1.13 303 65174.14 6.62 33.66 6.87- 0.98 404 60753.22 6.15 29.70 6.87- 0.90 505 55529.35 5.65 27.33 6.87- 0.81 606 48818.13 5.02 24.09 6.87- 0.74 707 44646.29 4.71 22.77 6.87- 0.68 808 41250.97 4.42 21.53 6.87- 0.62 909 37943.61 4.12 20.35 6.87- 0.49 1015 35111.94 3.88 19.70 ------------------------------------------------------------------------------------ 6.87- 0.49 1015 35111.94 3.88 19.70 Scale applied to data: s=0.422986 (maximum obs:2364142.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.105; Rsigma 0.059: data 1015 -> merged 638 With outlier rejection... Rint 0.094; Rsigma 0.058: data 993 -> merged 638 Rejected total: 22, method kkm 21, method Blessing 1 Completeness direct cell (a, b, c) = (6.884, 6.884, 5.976), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.486081, 6.884192 completeness table (Laue group: P4/m (tetra-c), Friedel couples are equivalent) range data theory redun '%' total 7.41 - 1.47 59 59 2.59 100.00 153 1.46 - 1.13 59 59 2.14 100.00 126 1.13 - 0.98 59 59 1.85 100.00 109 0.98 - 0.89 59 59 1.63 100.00 96 0.89 - 0.82 55 59 1.51 93.22 83 0.82 - 0.77 53 59 1.42 89.83 75 0.77 - 0.74 48 59 1.27 81.36 61 0.74 - 0.70 46 59 1.24 77.97 57 0.70 - 0.67 33 59 1.18 55.93 39 0.67 - 0.65 34 59 1.18 57.63 40 --------------------------------------------------------------- 7.41 - 0.65 505 590 1.66 85.59 839 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:21:15 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.380272 7.366633 7.425517 120.5228 120.4173 89.2690 993 Reflections read from file xs2212a.hkl 546 Reflections used for space-group determination (up to diffraction limit of 0.82A); mean (I/sigma) = 5.50 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 268 280 270 269 409 363 367 546 N (int>3sigma) = 0 36 35 51 32 61 88 88 132 Mean intensity = 0.0 0.6 0.6 0.9 0.5 0.7 21.8 24.6 22.0 Mean int/sigma = 0.0 1.6 1.6 2.3 1.5 1.8 5.2 6.0 5.5 Lattice type: P chosen Volume: 283.21 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 1.0000 Unitcell: 7.338 7.356 7.362 60.07 60.27 89.68 Niggli form: a.a = 53.842 b.b = 54.115 c.c = 54.206 b.c = 27.026 a.c = 26.790 a.b = 0.304 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.766 CUBIC F-lattice R(int) = 0.333 [ 436] Vol = 1132.8 Cell: 10.419 10.361 10.494 90.11 90.49 90.14 Volume: 1132.83 Matrix:-1.0000 -1.0000 -2.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.801 TETRAGONAL I-lattice R(int) = 0.127 [ 269] Vol = 566.4 Cell: 7.367 7.380 10.419 89.75 89.55 89.27 Volume: 566.41 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.442 TETRAGONAL I-lattice R(int) = 0.309 [ 280] Vol = 566.4 Cell: 7.338 7.356 10.494 89.73 89.58 89.68 Volume: 566.41 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.400 ORTHORHOMBIC F-lattice R(int) = 0.136 [ 257] Vol = 1132.8 Cell: 10.419 10.361 10.494 89.89 90.49 89.86 Volume: 1132.83 Matrix: 1.0000 1.0000 2.0000 1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.758 ORTHORHOMBIC I-lattice R(int) = 0.145 [ 271] Vol = 566.4 Cell: 10.419 7.380 7.367 89.27 89.55 89.75 Volume: 566.41 Matrix: 1.0000 1.0000 2.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.333 ORTHORHOMBIC I-lattice R(int) = 0.310 [ 301] Vol = 566.4 Cell: 7.338 7.356 10.494 90.27 90.42 89.68 Volume: 566.41 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.327 MONOCLINIC I-lattice R(int) = 0.088 [ 142] Vol = 566.4 Cell: 7.362 10.361 7.426 90.03 90.41 90.18 Volume: 566.41 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.487 MONOCLINIC I-lattice R(int) = 0.131 [ 134] Vol = 566.4 Cell: 7.380 10.419 7.367 90.45 90.73 89.75 Volume: 566.41 Matrix:-1.0000 0.0000 0.0000 1.0000 1.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.331 MONOCLINIC I-lattice R(int) = 0.328 [ 152] Vol = 566.4 Cell: 7.356 7.338 10.494 89.58 90.27 90.32 Volume: 566.41 Matrix: 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.306 MONOCLINIC I-lattice R(int) = 0.320 [ 230] Vol = 566.4 Cell: 7.338 7.356 10.494 89.73 90.42 90.32 Volume: 566.41 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.019 [ 33] Vol = 283.2 Cell: 7.338 7.356 7.362 60.07 60.27 89.68 Volume: 283.21 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 1.0000 Option [ 6] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 267 277 270 0 407 379 367 546 N (int>3sigma) = 0 31 32 51 0 57 85 91 132 Mean intensity = 0.0 0.5 0.5 0.9 0.0 0.7 20.4 24.1 22.0 Mean int/sigma = 0.0 1.5 1.6 2.3 0.0 1.8 5.0 5.8 5.5 Crystal system TETRAGONAL and Lattice type I selected Mean |E*E-1| = 3.724 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41/43 a-- -c- --d N 3 20 51 41 N I>3s 0 0 17 0 0.1 0.0 1.3 -0.0 0.6 0.3 3.2 0.2 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) I4(1)/amd 1 1 141 C N N N N 41 526 0.146 336 I4(1)/amd 4/mmm Tetragonal (1) x, y, z (2) -x+1/2,-y, z+1/2 (3) -y+1/4, x+3/4, z+1/4 (4) y+1/4,-x+1/4, z+3/4 (5) -x+1/2, y,-z+1/2 (6) x,-y,-z (7) y+1/4, x+3/4,-z+1/4 (8) -y+1/4,-x+1/4,-z+3/4 (9) -x,-y,-z (10) x+1/2, y,-z+1/2 (11) y+3/4,-x+1/4,-z+3/4 (12) -y+3/4, x+3/4,-z+1/4 (13) x+1/2,-y, z+1/2 (14) -x, y, z (15) -y+3/4,-x+1/4, z+3/4 (16) y+3/4, x+3/4, z+1/4 Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in I4(1)/amd REM I4(1)/amd (#141 in standard setting) CELL 0.71073 7.366633 7.380272 10.419462 89.7540 89.5503 89.2690 ZERR 1.00 0.006103 0.006434 0.026086 0.1634 0.1634 0.0690 LATT 2 SYMM -x+1/2,-y, z+1/2 SYMM -y+1/4, x+3/4, z+1/4 SYMM y+1/4,-x+1/4, z+3/4 SYMM -x+1/2, y,-z+1/2 SYMM x,-y,-z SYMM y+1/4, x+3/4,-z+1/4 SYMM -y+1/4,-x+1/4,-z+3/4 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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: P4/m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 2364143- 99512 100 98 63 1.6 330206.04 25.99 0.080 0.091 97606- 3116 118 109 63 1.7 19801.28 4.91 0.283 0.269 3103- 1516 122 115 63 1.8 2119.38 2.16 0.447 0.451 1500- 942 104 104 63 1.7 1179.92 1.51 0.503 0.527 938- 646 92 91 63 1.4 790.79 1.09 0.594 0.624 641- 446 93 92 63 1.5 537.16 1.03 0.540 0.571 442- 292 97 95 63 1.5 340.44 0.73 0.555 0.580 285- 137 101 101 63 1.6 209.06 0.62 0.712 0.821 137- 14 87 87 63 1.4 63.85 0.40 0.878 1.777 12- -872 101 101 71 1.4 -167.91 -0.22 0.969 2.166 ------------------------------------------------------------------------------------------- 2364143- -872 1015 993 638 1.6 35295.47 3.85 0.094 0.105 Statistics vs resolution - point group symmetry: P4/m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.43 175 164 63 2.6 86812.27 8.62 0.081 0.096 0.026 1.43-1.11 141 132 64 2.1 44234.56 4.64 0.091 0.099 0.054 1.11-0.96 115 114 63 1.8 34331.51 3.33 0.092 0.091 0.069 0.96-0.87 102 101 63 1.6 38430.38 3.89 0.111 0.127 0.071 0.87-0.80 91 91 63 1.4 23724.37 2.73 0.123 0.123 0.097 0.80-0.75 81 81 63 1.3 8647.71 1.71 0.126 0.126 0.135 0.75-0.70 81 81 63 1.3 18277.85 2.46 0.183 0.183 0.096 0.70-0.65 75 75 63 1.2 13198.14 2.04 0.031 0.031 0.125 0.65-0.60 73 73 63 1.2 15909.54 2.19 0.138 0.138 0.112 0.60-0.49 81 81 70 1.2 8466.99 1.57 0.137 0.137 0.159 ------------------------------------------------------------------------------------------------------ inf-0.49 1015 993 638 1.6 35295.47 3.85 0.094 0.105 0.058 inf-0.65 861 839 505 1.7 39572.33 4.22 0.092 0.103 0.054 Statistics vs resolution (taking redundancy into account) - point group symmetry: P4/m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.43 164 63 63 100.0 2.6 86812.27 13.33 0.081 0.018 1.43-1.11 132 64 64 100.0 2.1 44234.56 6.57 0.091 0.038 1.11-0.96 114 63 63 100.0 1.8 34331.51 4.10 0.092 0.057 0.96-0.87 101 64 63 98.4 1.6 38430.38 4.81 0.111 0.050 0.87-0.80 91 69 63 91.3 1.4 23724.37 3.19 0.123 0.087 0.80-0.75 81 75 63 84.0 1.3 8647.71 2.01 0.126 0.105 0.75-0.70 81 79 63 79.7 1.3 18277.85 2.82 0.183 0.075 0.70-0.65 75 113 63 55.8 1.2 13198.14 2.27 0.031 0.088 0.65-0.60 73 144 63 43.8 1.2 15909.54 2.55 0.138 0.067 0.60-0.49 81 631 70 11.1 1.2 8466.99 1.83 0.137 0.097 -------------------------------------------------------------------------------------------- inf-0.49 993 1373 638 46.5 1.6 35295.47 5.23 0.094 0.040 inf-0.65 839 590 505 85.6 1.7 39572.33 5.79 0.092 0.038 Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 0.0 1.0 0.0 1.0 0.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: 0.0 1.0 0.0 1.0 0.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.054817 0.078744 -0.008726 ( 0.000063 0.000086 0.000046 ) 0.078756 0.051232 -0.013612 ( 0.000051 0.000070 0.000037 ) -0.008114 -0.020301 -0.065983 ( 0.000054 0.000074 0.000039 ) M - matrix: 0.009273 -0.000117 -0.000058 ( 0.000011 0.000009 0.000005 ) -0.000117 0.009237 -0.000045 ( 0.000009 0.000016 0.000007 ) -0.000058 -0.000045 0.004615 ( 0.000005 0.000007 0.000005 ) Constraint UB - matrix: -0.054817 0.078744 -0.008726 ( 0.000063 0.000086 0.000046 ) 0.078756 0.051232 -0.013612 ( 0.000051 0.000070 0.000037 ) -0.008114 -0.020301 -0.065983 ( 0.000054 0.000074 0.000039 ) M - matrix: 0.009293 0.000000 0.000000 ( 0.000004 0.000000 0.000000 ) 0.000000 0.009293 0.000000 ( 0.000000 0.000004 0.000000 ) 0.000000 0.000000 0.004640 ( 0.000000 0.000000 0.000003 ) unit cell: 7.367(5) 7.381(5) 10.441(6) 89.60(5) 89.48(5) 89.27(6) V = 567.6(7) unit cell: 7.3747(16) 7.3747(16) 10.437(3) 90.0 90.0 90.0 V = 567.6(2) Laue class changed... Laue class: 4/mmm - Friedel mate is equivalent Point group: 4/mmm Lattice type: I-lattice (extinction condition applied) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-558.0000 max=6109867.0000 PROFFIT INFO: signal sum lp corr: min=-578.6852 max=792081.7013 PROFFIT INFO: background sum: min=160.0000 max=5938.0000 PROFFIT INFO: background sum sig2: min=520.0000 max=4997.0000 PROFFIT INFO: num of signal pixels: min=50 max=497 PROFFIT INFO: Inet: min=-925.8964 max=1267330.7500 PROFFIT INFO: sig(Inet): min=63.9097 max=17698.8184 PROFFIT INFO: Inet/sig(Inet): min=-1.69 max=164.82 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 226 780 1156 1326 1422 1624 1732 1804 1942 2018 2034 Percent 11.1 38.3 56.8 65.2 69.9 79.8 85.2 88.7 95.5 99.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1017 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 1017 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1267331- 116930 101 314971.59 70.65 100.00 114860- 3412 101 25511.01 18.09 100.00 3380- 1771 101 2474.10 6.07 94.06 1753- 1055 101 1334.30 3.16 37.62 1052- 702 101 853.81 1.92 7.92 701- 470 101 586.91 1.45 8.91 468- 262 101 357.47 1.01 1.98 259- 105 101 176.33 0.51 0.00 105- -8 101 45.55 0.17 0.00 -9- -926 108 -203.76 -0.39 0.00 ------------------------------------------------------------------------------------ 1267331- -926 1017 34371.10 10.19 34.81 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.59 101 70017.34 12.96 67.33 1.59- 1.23 101 57041.35 18.65 50.50 1.23- 1.05 101 66214.85 20.13 66.34 1.05- 0.95 101 29202.27 9.36 19.80 0.95- 0.87 101 41822.65 13.04 50.50 0.87- 0.80 101 18295.77 6.42 23.76 0.80- 0.75 101 17343.30 5.74 22.77 0.75- 0.71 101 21625.49 7.37 16.83 0.71- 0.67 101 21551.20 7.31 25.74 0.67- 0.63 108 2785.87 1.52 6.48 ------------------------------------------------------------------------------------ 6.01- 0.63 1017 34371.10 10.19 34.81 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:21:15 2019 Sorting 1017 observations 62 unique observations with > 7.00 F2/sig(F2) 1017 observations in 1 runs Run # start # end # total # 1 0 102 103 Total number of frames 103 Maximum number of 62 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1017 observations in 1 runs Run # start # end # total # 1 0 51 52 Total number of frames 52 223 observations > 7.00 F2/sig(F2) 223 observations in 1 runs Run # start # end # total # 1 0 50 51 Total number of frames 51 Frame #25 of 51 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: 3.1 (Out of 223 removed 22 = 201, unique = 64) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m2/m2/m 201 observations in 1 runs Run # start # end # total # 1 0 50 51 Total number of frames 51 Frame #25 of 51 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 64 unique data precomputed (should be 64) 64 unique data with 201 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.1 (Out of 201 removed 0 = 201, unique = 64) 64 unique data precomputed (should be 64) 64 unique data with 201 observations RMS deviation of equivalent data = 0.12456 Rint = 0.09649 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.09649, wR= 0.13498 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09788, wR= 0.13235, Acormin=0.634, Acormax=0.916, Acor_av=0.751 F test: Probability=0.000, F= 0.937 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07135, wR= 0.09782, Acormin=0.507, Acormax=1.268, Acor_av=0.817 F test: Probability=0.999, F= 1.722 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07227, wR= 0.09967, Acormin=0.530, Acormax=1.057, Acor_av=0.690 F test: Probability=0.000, F= 0.929 Trying model 4 (ne=4, no=1)... Results: Rint= 0.04392, wR= 0.06306, Acormin=0.423, Acormax=1.230, Acor_av=0.783 F test: Probability=1.000, F= 2.455 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03848, wR= 0.05376, Acormin=0.420, Acormax=1.405, Acor_av=0.841 F test: Probability=0.864, F= 1.227 Trying model 6 (ne=6, no=0)... Results: Rint= 0.05753, wR= 0.06745, Acormin=0.595, Acormax=1.856, Acor_av=0.817 F test: Probability=0.000, F= 0.534 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03330, wR= 0.04268, Acormin=0.499, Acormax=1.798, Acor_av=0.884 F test: Probability=0.990, F= 1.552 Trying model 8 (ne=6, no=3)... Results: Rint= 0.03239, wR= 0.04008, Acormin=0.495, Acormax=1.634, Acor_av=0.897 F test: Probability=0.000, F= 0.988 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02620, wR= 0.03689, Acormin=0.492, Acormax=1.509, Acor_av=0.910 F test: Probability=0.924, F= 1.343 Final absorption model (ne=6, no=1): Rint= 0.03330, Acormin=0.499, Acormax=1.798, Acor_av=0.884 Combined refinement in use Rint: 0.09978 There are 50 active scales (one needs to be fixed) Refinement control: frame scale #43 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 1 (30 parameters) Refinement control: 79 pars with 3160 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.12456 Using Levenberg-Marquardt: 0.00010 New wR= 0.03425 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.02714 Rint for all data: 0.09978 with corrections 0.03175 0 observations identified as outliers and rejected Cycle 2 wR= 0.03425 Using Levenberg-Marquardt: 0.00001 New wR= 0.03554 Using Levenberg-Marquardt: 0.00010 New wR= 0.03473 Using Levenberg-Marquardt: 0.00100 New wR= 0.03213 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.02331 Rint for all data: 0.09978 with corrections 0.02835 0 observations identified as outliers and rejected Cycle 3 wR= 0.03213 Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 New wR= 0.03930 Using Levenberg-Marquardt: 0.01000 New wR= 0.02997 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.02252 Rint for all data: 0.09978 with corrections 0.02758 0 observations identified as outliers and rejected Cycle 4 wR= 0.02997 Using Levenberg-Marquardt: 0.00100 New wR= 0.02987 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.02241 Rint for all data: 0.09978 with corrections 0.02782 0 observations identified as outliers and rejected Cycle 5 wR= 0.02987 Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 New wR= 0.02991 Using Levenberg-Marquardt: 0.01000 New wR= 0.02935 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.02247 Rint for all data: 0.09978 with corrections 0.02794 0 observations identified as outliers and rejected Final wR= 0.02935 Final frame scales: Min= 0.9624 Max= 1.3954 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics There are 50 active scales (one needs to be fixed) Refinement control: frame scale #43 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 0 (27 parameters) Refinement control: 76 pars with 2926 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.21682 Using Levenberg-Marquardt: 0.00010 New wR= 0.07553 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.05059 Rint for all data: 0.09978 with corrections 0.05461 0 observations identified as outliers and rejected Cycle 2 wR= 0.07553 Using Levenberg-Marquardt: 0.00001 New wR= 0.04180 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.04413 Rint for all data: 0.09978 with corrections 0.04995 0 observations identified as outliers and rejected Cycle 3 wR= 0.04180 Using Levenberg-Marquardt: 0.00000 New wR= 0.03471 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.03026 Rint for all data: 0.09978 with corrections 0.03507 0 observations identified as outliers and rejected Cycle 4 wR= 0.03471 Using Levenberg-Marquardt: 0.00000 New wR= 0.03278 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.02885 Rint for all data: 0.09978 with corrections 0.03381 0 observations identified as outliers and rejected Cycle 5 wR= 0.03278 Using Levenberg-Marquardt: 0.00000 New wR= 0.03404 Using Levenberg-Marquardt: 0.00000 New wR= 0.03404 Using Levenberg-Marquardt: 0.00000 New wR= 0.03404 Using Levenberg-Marquardt: 0.00001 New wR= 0.03402 Using Levenberg-Marquardt: 0.00010 New wR= 0.03387 Using Levenberg-Marquardt: 0.00100 New wR= 0.03329 Using Levenberg-Marquardt: 0.01000 New wR= 0.03277 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.02876 Rint for all data: 0.09978 with corrections 0.03369 Final wR= 0.03277 Final frame scales: Min= 0.8686 Max= 1.4557 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics There are 50 active scales (one needs to be fixed) Refinement control: frame scale #43 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 1 (17 parameters) Refinement control: 66 pars with 2211 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22498 Using Levenberg-Marquardt: 0.00010 New wR= 0.07731 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.05070 Rint for all data: 0.09978 with corrections 0.05462 0 observations identified as outliers and rejected Cycle 2 wR= 0.07731 Using Levenberg-Marquardt: 0.00001 New wR= 0.04014 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.03522 Rint for all data: 0.09978 with corrections 0.03997 0 observations identified as outliers and rejected Cycle 3 wR= 0.04014 Using Levenberg-Marquardt: 0.00000 New wR= 0.03655 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.03225 Rint for all data: 0.09978 with corrections 0.03682 0 observations identified as outliers and rejected Cycle 4 wR= 0.03655 Using Levenberg-Marquardt: 0.00000 New wR= 0.03516 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.03003 Rint for all data: 0.09978 with corrections 0.03466 0 observations identified as outliers and rejected Cycle 5 wR= 0.03516 Using Levenberg-Marquardt: 0.00000 New wR= 0.03563 Using Levenberg-Marquardt: 0.00000 New wR= 0.03563 Using Levenberg-Marquardt: 0.00000 New wR= 0.03563 Using Levenberg-Marquardt: 0.00001 New wR= 0.03563 Using Levenberg-Marquardt: 0.00010 New wR= 0.03563 Using Levenberg-Marquardt: 0.00100 New wR= 0.03559 Using Levenberg-Marquardt: 0.01000 New wR= 0.03545 Using Levenberg-Marquardt: 0.10000 New wR= 0.03524 Using Levenberg-Marquardt: 1.00000 New wR= 0.03515 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.09649 with corrections 0.02998 Rint for all data: 0.09978 with corrections 0.03461 Final wR= 0.03515 Final frame scales: Min= 0.7652 Max= 1.3216 Final absorption correction factors: Amin= 0.1353 Amax= 1.8437 PROFFIT INFO: Inet (after scale3 abspack): min=-2141.4844 max=1014230.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=60.7812 max=18770.6191 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 6, Friedel: 1 Min/max for: run:1/1 frame:1/103 1017 reflections read from tmp file 78 reflections are rejected (14 as outliers, 64 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8+ Number of groups: 0 86 109 75 14 9 0 2 Initial Chi^2= 0.64305 Cycle 1, Chi^2= 1.04267 Current error model SIG(F2)^2 = 88.36*I_RAW + 8.06*I_BACK+(0.03389*)^2 Cycle 2, Chi^2= 1.03719 Current error model SIG(F2)^2 = 105.30*I_RAW + 4.59*I_BACK+(0.03141*)^2 Cycle 3, Chi^2= 1.01646 Current error model SIG(F2)^2 = 113.44*I_RAW + 3.36*I_BACK+(0.03232*)^2 Cycle 4, Chi^2= 1.00919 Current error model SIG(F2)^2 = 117.98*I_RAW + 2.73*I_BACK+(0.03196*)^2 Cycle 5, Chi^2= 1.00382 Current error model SIG(F2)^2 = 119.96*I_RAW + 2.47*I_BACK+(0.03218*)^2 Cycle 6, Chi^2= 1.00197 Current error model SIG(F2)^2 = 120.97*I_RAW + 2.35*I_BACK+(0.03210*)^2 Cycle 7, Chi^2= 1.00077 Current error model SIG(F2)^2 = 121.38*I_RAW + 2.30*I_BACK+(0.03215*)^2 Cycle 8, Chi^2= 1.00040 Current error model SIG(F2)^2 = 121.59*I_RAW + 2.27*I_BACK+(0.03213*)^2 Cycle 9, Chi^2= 1.00015 Current error model SIG(F2)^2 = 121.67*I_RAW + 2.26*I_BACK+(0.03214*)^2 Final Chi^2= 1.00015 Final error model SIG(F2)^2 = 121.67*I_RAW + 2.26*I_BACK+(0.03214*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1014230- 92918 101 315151.64 24.11 100.00 92640- 3597 101 22729.55 10.41 98.02 3515- 1766 101 2446.46 4.71 88.12 1750- 981 101 1297.35 3.00 41.58 980- 631 101 782.63 2.19 6.93 630- 421 101 527.79 1.85 5.94 420- 248 101 331.30 1.58 4.95 244- 98 101 166.03 1.13 0.00 98- -8 101 44.41 0.46 0.00 -9- -2141 108 -241.16 -0.80 0.00 ------------------------------------------------------------------------------------ 1014230- -2141 1017 34085.69 4.82 34.32 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.59 101 69351.75 7.68 68.32 1.59- 1.23 101 64112.89 6.59 50.50 1.23- 1.05 101 62960.80 7.46 68.32 1.05- 0.95 101 30878.26 4.01 19.80 0.95- 0.87 101 38455.50 6.33 48.51 0.87- 0.80 101 18157.11 3.42 21.78 0.80- 0.75 101 16572.42 3.34 20.79 0.75- 0.71 101 21161.48 4.25 17.82 0.71- 0.67 101 18815.34 4.09 25.74 0.67- 0.63 108 2575.25 1.32 3.70 ------------------------------------------------------------------------------------ 6.01- 0.63 1017 34085.69 4.82 34.32 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.59 101 69351.75 7.68 68.32 6.01- 1.23 202 66732.32 7.14 59.41 6.01- 1.05 303 65475.14 7.24 62.38 6.01- 0.95 404 56825.92 6.44 51.73 6.01- 0.87 505 53151.84 6.41 51.09 6.01- 0.80 606 47319.38 5.92 46.20 6.01- 0.75 707 42926.96 5.55 42.57 6.01- 0.71 808 40206.28 5.39 39.48 6.01- 0.67 909 37829.50 5.24 37.95 6.01- 0.63 1017 34085.69 4.82 34.32 ------------------------------------------------------------------------------------ 6.01- 0.63 1017 34085.69 4.82 34.32 Scale applied to data: s=0.985969 (maximum obs:1014230.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.035; Rsigma 0.048: data 1017 -> merged 360 With outlier rejection... Rint 0.033; Rsigma 0.048: data 1001 -> merged 360 Rejected total: 16, method kkm 16, method Blessing 0 Completeness direct cell (a, b, c) = (7.375, 7.375, 10.437), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627802, 6.022874 completeness table (Laue group: I4/mmm (tetra-c), Friedel couples are equivalent) range data theory redun '%' total 7.41 - 1.59 33 34 3.12 97.06 103 1.59 - 1.20 33 34 3.33 97.06 110 1.20 - 1.02 34 34 3.21 100.00 109 1.02 - 0.91 34 34 3.18 100.00 108 0.91 - 0.85 34 34 2.82 100.00 96 0.85 - 0.80 34 34 2.91 100.00 99 0.80 - 0.75 33 34 2.73 97.06 90 0.75 - 0.72 33 34 2.52 97.06 83 0.72 - 0.68 31 34 2.55 91.18 79 0.68 - 0.65 37 41 2.38 90.24 88 --------------------------------------------------------------- 7.41 - 0.65 336 347 2.87 96.83 965 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:21:15 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.380272 7.366633 7.425517 120.5228 120.4173 89.2690 993 Reflections read from file xs2212a.hkl 546 Reflections used for space-group determination (up to diffraction limit of 0.82A); mean (I/sigma) = 5.50 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 268 280 270 269 409 363 367 546 N (int>3sigma) = 0 36 35 51 32 61 88 88 132 Mean intensity = 0.0 0.6 0.6 0.9 0.5 0.7 21.8 24.6 22.0 Mean int/sigma = 0.0 1.6 1.6 2.3 1.5 1.8 5.2 6.0 5.5 Lattice type: P chosen Volume: 283.21 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 1.0000 Unitcell: 7.338 7.356 7.362 60.07 60.27 89.68 Niggli form: a.a = 53.842 b.b = 54.115 c.c = 54.206 b.c = 27.026 a.c = 26.790 a.b = 0.304 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.766 CUBIC F-lattice R(int) = 0.333 [ 436] Vol = 1132.8 Cell: 10.419 10.361 10.494 90.11 90.49 90.14 Volume: 1132.83 Matrix:-1.0000 -1.0000 -2.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.801 TETRAGONAL I-lattice R(int) = 0.127 [ 269] Vol = 566.4 Cell: 7.367 7.380 10.419 89.75 89.55 89.27 Volume: 566.41 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.442 TETRAGONAL I-lattice R(int) = 0.309 [ 280] Vol = 566.4 Cell: 7.338 7.356 10.494 89.73 89.58 89.68 Volume: 566.41 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.400 ORTHORHOMBIC F-lattice R(int) = 0.136 [ 257] Vol = 1132.8 Cell: 10.419 10.361 10.494 89.89 90.49 89.86 Volume: 1132.83 Matrix: 1.0000 1.0000 2.0000 1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.758 ORTHORHOMBIC I-lattice R(int) = 0.145 [ 271] Vol = 566.4 Cell: 10.419 7.380 7.367 89.27 89.55 89.75 Volume: 566.41 Matrix: 1.0000 1.0000 2.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.333 ORTHORHOMBIC I-lattice R(int) = 0.310 [ 301] Vol = 566.4 Cell: 7.338 7.356 10.494 90.27 90.42 89.68 Volume: 566.41 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.327 MONOCLINIC I-lattice R(int) = 0.088 [ 142] Vol = 566.4 Cell: 7.362 10.361 7.426 90.03 90.41 90.18 Volume: 566.41 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.487 MONOCLINIC I-lattice R(int) = 0.131 [ 134] Vol = 566.4 Cell: 7.380 10.419 7.367 90.45 90.73 89.75 Volume: 566.41 Matrix:-1.0000 0.0000 0.0000 1.0000 1.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.331 MONOCLINIC I-lattice R(int) = 0.328 [ 152] Vol = 566.4 Cell: 7.356 7.338 10.494 89.58 90.27 90.32 Volume: 566.41 Matrix: 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.306 MONOCLINIC I-lattice R(int) = 0.320 [ 230] Vol = 566.4 Cell: 7.338 7.356 10.494 89.73 90.42 90.32 Volume: 566.41 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.019 [ 33] Vol = 283.2 Cell: 7.338 7.356 7.362 60.07 60.27 89.68 Volume: 283.21 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 1.0000 Option [ 6] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 267 277 270 0 407 379 367 546 N (int>3sigma) = 0 31 32 51 0 57 85 91 132 Mean intensity = 0.0 0.5 0.5 0.9 0.0 0.7 20.4 24.1 22.0 Mean int/sigma = 0.0 1.5 1.6 2.3 0.0 1.8 5.0 5.8 5.5 Crystal system TETRAGONAL and Lattice type I selected Mean |E*E-1| = 3.724 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41/43 a-- -c- --d N 3 20 51 41 N I>3s 0 0 17 0 0.1 0.0 1.3 -0.0 0.6 0.3 3.2 0.2 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) I4(1)/amd 1 1 141 C N N N N 41 526 0.146 336 I4(1)/amd 4/mmm Tetragonal (1) x, y, z (2) -x+1/2,-y, z+1/2 (3) -y+1/4, x+3/4, z+1/4 (4) y+1/4,-x+1/4, z+3/4 (5) -x+1/2, y,-z+1/2 (6) x,-y,-z (7) y+1/4, x+3/4,-z+1/4 (8) -y+1/4,-x+1/4,-z+3/4 (9) -x,-y,-z (10) x+1/2, y,-z+1/2 (11) y+3/4,-x+1/4,-z+3/4 (12) -y+3/4, x+3/4,-z+1/4 (13) x+1/2,-y, z+1/2 (14) -x, y, z (15) -y+3/4,-x+1/4, z+3/4 (16) y+3/4, x+3/4, z+1/4 Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in I4(1)/amd REM I4(1)/amd (#141 in standard setting) CELL 0.71073 7.366633 7.380272 10.419462 89.7540 89.5503 89.2690 ZERR 1.00 0.006103 0.006434 0.026086 0.1634 0.1634 0.0690 LATT 2 SYMM -x+1/2,-y, z+1/2 SYMM -y+1/4, x+3/4, z+1/4 SYMM y+1/4,-x+1/4, z+3/4 SYMM -x+1/2, y,-z+1/2 SYMM x,-y,-z SYMM y+1/4, x+3/4,-z+1/4 SYMM -y+1/4,-x+1/4,-z+3/4 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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: I4/mmm # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 971092- 120986 87 86 36 2.4 349785.92 25.02 0.027 0.032 120109- 3864 101 100 36 2.8 37148.73 12.27 0.043 0.047 3689- 1781 116 114 36 3.2 2571.64 4.76 0.130 0.143 1730- 911 115 113 36 3.1 1161.97 2.73 0.226 0.258 910- 565 113 112 36 3.1 726.88 1.99 0.256 0.281 561- 342 109 109 36 3.0 437.96 1.70 0.379 0.439 337- 237 116 111 36 3.1 287.32 1.37 0.454 0.554 231- 79 89 89 36 2.5 142.27 0.94 0.622 0.788 77- -32 90 89 36 2.5 20.28 0.26 0.920 2.935 -33- -1495 81 78 36 2.2 -213.57 -0.57 0.721 0.872 ------------------------------------------------------------------------------------------- 971092- -1495 1017 1001 360 2.8 34345.44 4.85 0.033 0.038 Statistics vs resolution - point group symmetry: I4/mmm resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.51 117 115 36 3.2 109339.05 9.66 0.026 0.032 0.035 1.46-1.17 117 117 36 3.3 50612.79 6.34 0.023 0.024 0.041 1.15-1.01 118 117 36 3.3 11746.36 3.45 0.049 0.054 0.060 1.01-0.89 115 113 36 3.1 33643.31 4.78 0.025 0.032 0.047 0.89-0.82 103 100 36 2.8 47074.34 7.02 0.038 0.042 0.050 0.82-0.78 103 102 36 2.8 15224.41 3.05 0.033 0.033 0.066 0.78-0.73 97 97 36 2.7 8410.61 1.95 0.105 0.101 0.085 0.73-0.69 93 93 36 2.6 24788.26 5.43 0.038 0.039 0.066 0.69-0.66 89 84 36 2.3 12686.11 2.94 0.056 0.061 0.084 0.66-0.63 65 63 36 1.8 4142.55 1.61 0.273 0.276 0.144 ------------------------------------------------------------------------------------------------------ inf-0.63 1017 1001 360 2.8 34345.44 4.85 0.033 0.038 0.048 inf-0.66 978 963 335 2.9 35439.29 4.96 0.032 0.037 0.047 Statistics vs resolution (taking redundancy into account) - point group symmetry: I4/mmm resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.51 115 37 36 97.3 3.2 109339.05 18.29 0.026 0.020 1.46-1.17 117 37 36 97.3 3.3 50612.79 11.39 0.023 0.025 1.15-1.01 117 36 36 100.0 3.3 11746.36 6.26 0.049 0.035 1.01-0.89 113 36 36 100.0 3.1 33643.31 8.88 0.025 0.026 0.89-0.82 100 36 36 100.0 2.8 47074.34 11.85 0.038 0.031 0.82-0.78 102 36 36 100.0 2.8 15224.41 5.10 0.033 0.040 0.78-0.73 97 38 36 94.7 2.7 8410.61 3.19 0.105 0.050 0.73-0.69 93 37 36 97.3 2.6 24788.26 8.79 0.038 0.040 0.69-0.66 84 39 36 92.3 2.3 12686.11 4.85 0.056 0.053 0.66-0.63 63 60 36 60.0 1.8 4142.55 2.14 0.273 0.107 -------------------------------------------------------------------------------------------- inf-0.63 1001 392 360 91.8 2.8 34345.44 8.54 0.033 0.029 inf-0.66 963 344 335 97.4 2.9 35439.29 8.77 0.032 0.029 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm started DELETE INFO: Deleting rpi files... (D:\Data\xs2212a\tmp\xs2212a_proffitpea*.rpi) DELETE INFO: Deleting tab files... (D:\Data\xs2212a\tmp\xs2212a_proffitpea*.tab) DELETE INFO: Deleting tabbin files... (D:\Data\xs2212a\tmp\xs2212a_proffitpea*.tabbin) DELETE INFO: Deleting rrpprof files... (D:\Data\xs2212a\tmp\xs2212a*.rrpprof) DELETE INFO: Deleting rrpprofinfo files... (D:\Data\xs2212a\tmp\xs2212a*.rrpprofinfo) DELETE INFO: Deleting bbm files... (D:\Data\xs2212a\tmp\xs2212a*.bbm) DELETE INFO: Deleting pcorr files... (D:\Data\xs2212a\tmp\xs2212a*.pcorr) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\tmp\xs2212a*.dat) DELETE INFO: Deleting ppc2 files... (D:\Data\xs2212a\tmp\xs2212a*.ppc2) DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:25:45 2019) ID: 3668; threads 40; handles 809; mem 514628.00 (1204700.00)kB; time: 1w 4d 22h 36m 32s MEMORY INFO: Memory PF:72.0, Ph:520.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:502.6,peak PF: 700.2, WS: 470.8, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:77.0, Ph:522.0, V:1178.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:504.4,peak PF: 700.2, WS: 472.6, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:25:45 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000099 0.000060 0.000091 ) 0.064809 0.092374 0.027273 ( 0.000086 0.000052 0.000080 ) 0.045523 0.057900 0.132205 ( 0.000104 0.000064 0.000096 ) 7.38096 ( 0.00646 ) 7.36649 ( 0.00616 ) 7.42630 ( 0.00643 ) 120.52449 ( 0.09016 ) 120.40327 ( 0.09177 ) 89.27095 ( 0.06938 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 44 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 aP Cross checking gral lattice... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:25:45 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000099 0.000060 0.000091 ) 0.064809 0.092374 0.027273 ( 0.000086 0.000052 0.000080 ) 0.045523 0.057900 0.132205 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013920 0.004592 0.009315 ( 0.000023 0.000013 0.000018 ) 0.004592 0.014009 0.009368 ( 0.000013 0.000013 0.000013 ) 0.009315 0.009368 0.018528 ( 0.000018 0.000013 0.000026 ) unit cell: 7.381(6) 7.366(6) 7.426(6) 120.52(9) 120.40(9) 89.27(7) V = 283.3(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 219 peaks identified as outliers and rejected 219 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 219 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 219 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.78 | 22 | 0.982 ( 0.055) | 1.030 ( 0.146) | 1.095 ( 0.275) | 0.78- 0.69 | 22 | 0.977 ( 0.046) | 0.946 ( 0.104) | 1.312 ( 0.509) | 0.69- 0.63 | 21 | 0.945 ( 0.035) | 0.924 ( 0.096) | 1.289 ( 0.448) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 219 | 0.932 ( 0.177) | 0.943 ( 0.156) | 1.081 ( 0.812) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 203 obs out of 219 (total:219,skipped:0) (92.69%) UB - matrix: 0.087434 -0.046196 0.017570 ( 0.000091 0.000059 0.000090 ) 0.064796 0.092239 0.027378 ( 0.000081 0.000053 0.000080 ) 0.045563 0.057572 0.131881 ( 0.000106 0.000069 0.000104 ) M - matrix: 0.013919 0.004561 0.009319 ( 0.000021 0.000013 0.000018 ) 0.004561 0.013957 0.009306 ( 0.000013 0.000014 0.000014 ) 0.009319 0.009306 0.018451 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.371(6) 7.446(7) 120.46(9) 120.59(9) 89.13(7) V = 284.4(4) OTKP changes: 204 1 1 1 OTKP changes: 204 1 1 1 OTKP changes: 204 1 1 1 UB - matrix: 0.087501 -0.046094 0.017420 ( 0.000094 0.000061 0.000091 ) 0.064708 0.092378 0.027215 ( 0.000085 0.000055 0.000082 ) 0.045710 0.057894 0.132176 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013933 0.004591 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004591 0.014010 0.009363 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009363 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 207 obs out of 219 (total:219,skipped:0) (94.52%) unit cell: 7.382(6) 7.366(6) 7.433(7) 120.53(9) 120.47(9) 89.22(7) V = 283.4(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1310 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087501 -0.046094 0.017420 ( 0.000094 0.000061 0.000091 ) 0.064708 0.092378 0.027215 ( 0.000085 0.000055 0.000082 ) 0.045709 0.057894 0.132176 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013933 0.004591 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004591 0.014010 0.009363 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009363 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 207 obs out of 219 (total:219,skipped:0) (94.52%) unit cell: 7.382(6) 7.366(6) 7.433(7) 120.53(9) 120.47(9) 89.22(7) V = 283.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 211 obs out of 219 (total:219,skipped:0) (96.35%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.636 ( 2.376) | 2.60- 1.75 | 21 | 0.821 ( 0.087) | 0.812 ( 0.151) | 0.733 ( 0.327) | 1.75- 1.57 | 21 | 0.857 ( 0.091) | 0.890 ( 0.149) | 0.684 ( 0.234) | 1.56- 1.35 | 21 | 0.928 ( 0.073) | 0.993 ( 0.132) | 1.069 ( 0.542) | 1.35- 1.16 | 21 | 0.965 ( 0.067) | 1.042 ( 0.106) | 0.958 ( 0.392) | 1.16- 1.00 | 21 | 0.933 ( 0.078) | 0.961 ( 0.177) | 0.964 ( 0.398) | 1.00- 0.88 | 21 | 0.969 ( 0.078) | 1.009 ( 0.127) | 1.164 ( 0.518) | 0.88- 0.79 | 21 | 0.983 ( 0.049) | 1.027 ( 0.126) | 1.176 ( 0.357) | 0.79- 0.72 | 21 | 0.979 ( 0.042) | 0.956 ( 0.118) | 1.254 ( 0.467) | 0.69- 0.63 | 24 | 0.945 ( 0.039) | 0.929 ( 0.099) | 1.289 ( 0.477) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 213 | 0.938 ( 0.191) | 0.946 ( 0.157) | 1.095 ( 0.888) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=17, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=17, start=1, end=17, Data range for background initialization of run 2 more narrow than requested (is:17,should:25) BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb PROFFITPEAK info: 113 peaks in the peak location table UB fit with 19 obs out of 61 (total:61,skipped:0) (31.15%) UB - matrix: 0.086087 -0.047116 0.014612 ( 0.001335 0.000688 0.001469 ) 0.062186 0.091858 0.025803 ( 0.001113 0.000574 0.001225 ) 0.045548 0.057646 0.132646 ( 0.002111 0.001089 0.002323 ) M - matrix: 0.013353 0.004282 0.008904 ( 0.000330 0.000191 0.000336 ) 0.004282 0.013981 0.009328 ( 0.000191 0.000176 0.000238 ) 0.008904 0.009328 0.018474 ( 0.000336 0.000238 0.000621 ) unit cell: 7.45(9) 7.37(8) 7.39(13) 121(2) 120(2) 88.7(9) V = 287(8) UB fit with 19 obs out of 61 (total:61,skipped:0) (31.15%) UB - matrix: 0.086087 -0.047116 0.014612 ( 0.001335 0.000688 0.001469 ) 0.062186 0.091858 0.025803 ( 0.001113 0.000574 0.001225 ) 0.045548 0.057646 0.132646 ( 0.002111 0.001089 0.002323 ) M - matrix: 0.013353 0.004282 0.008904 ( 0.000330 0.000191 0.000336 ) 0.004282 0.013981 0.009328 ( 0.000191 0.000176 0.000238 ) 0.008904 0.009328 0.018474 ( 0.000336 0.000238 0.000621 ) unit cell: 7.45(9) 7.37(8) 7.39(13) 121(2) 120(2) 88.7(9) V = 287(8) OTKP changes: 15 1 1 1 OTKP changes: 15 1 1 1 OTKP changes: 15 1 1 1 UB - matrix: 0.087964 -0.044889 0.015395 ( 0.000346 0.000205 0.000398 ) 0.062784 0.093047 0.025815 ( 0.000364 0.000215 0.000419 ) 0.047667 0.056882 0.133297 ( 0.000362 0.000214 0.000416 ) M - matrix: 0.013952 0.004605 0.009329 ( 0.000084 0.000049 0.000069 ) 0.004605 0.013908 0.009293 ( 0.000049 0.000050 0.000057 ) 0.009329 0.009293 0.018672 ( 0.000069 0.000057 0.000114 ) UB fit with 57 obs out of 61 (total:61,skipped:0) (93.44%) unit cell: 7.36(2) 7.36(3) 7.35(3) 120.0(4) 120.2(4) 89.8(3) V = 281(2) UB fit with 57 obs out of 61 (total:61,skipped:0) (93.44%) UB - matrix: 0.087965 -0.044889 0.015396 ( 0.000346 0.000205 0.000399 ) 0.062785 0.093047 0.025816 ( 0.000364 0.000215 0.000419 ) 0.047666 0.056882 0.133297 ( 0.000362 0.000214 0.000417 ) M - matrix: 0.013952 0.004605 0.009329 ( 0.000084 0.000049 0.000069 ) 0.004605 0.013908 0.009293 ( 0.000049 0.000050 0.000057 ) 0.009329 0.009293 0.018672 ( 0.000069 0.000057 0.000114 ) unit cell: 7.36(2) 7.36(3) 7.35(3) 120.0(4) 120.2(4) 89.8(3) V = 281(2) OTKP changes: 16 1 1 1 OTKP changes: 16 1 1 1 OTKP changes: 16 1 1 1 OTKP changes: 16 1 1 1 OTKP changes: 16 1 1 1 OTKP changes: 16 1 1 1 61 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Run 2 Omega scan: (-49.000 - -32.000,17 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 377 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 57 obs out of 61 (total:61,skipped:0) (93.44%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=17, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=17, start=1, end=17, Data range for background initialization of run 2 more narrow than requested (is:17,should:25) BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb 0 of 41 peaks identified as outliers and rejected 41 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 41 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 41 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.12- 2.58 | 4 | 0.904 ( 0.086) | 0.920 ( 0.125) | 0.788 ( 0.150) | 2.39- 2.12 | 4 | 0.858 ( 0.101) | 0.880 ( 0.125) | 0.708 ( 0.225) | 2.10- 1.74 | 4 | 0.912 ( 0.099) | 0.885 ( 0.113) | 0.758 ( 0.392) | 1.64- 1.56 | 4 | 0.943 ( 0.032) | 0.972 ( 0.061) | 0.700 ( 0.171) | 1.45- 1.22 | 4 | 0.950 ( 0.053) | 0.972 ( 0.052) | 0.885 ( 0.279) | 1.22- 1.14 | 4 | 0.978 ( 0.044) | 1.011 ( 0.110) | 1.166 ( 0.641) | 1.09- 1.00 | 4 | 0.898 ( 0.066) | 0.988 ( 0.056) | 0.695 ( 0.136) | 1.00- 0.89 | 4 | 0.944 ( 0.043) | 0.931 ( 0.071) | 1.005 ( 0.308) | 0.88- 0.86 | 4 | 0.949 ( 0.064) | 0.941 ( 0.101) | 1.332 ( 0.402) | 0.78- 0.68 | 5 | 0.944 ( 0.029) | 0.929 ( 0.070) | 1.197 ( 0.389) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.12- 0.68 | 41 | 0.928 ( 0.074) | 0.942 ( 0.101) | 0.930 ( 0.411) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 41 obs out of 41 (total:41,skipped:0) (100.00%) UB - matrix: 0.087819 -0.044890 0.015337 ( 0.000213 0.000126 0.000246 ) 0.063101 0.093544 0.026085 ( 0.000222 0.000132 0.000256 ) 0.047847 0.056910 0.133302 ( 0.000261 0.000154 0.000301 ) M - matrix: 0.013983 0.004683 0.009371 ( 0.000053 0.000031 0.000047 ) 0.004683 0.014004 0.009338 ( 0.000031 0.000032 0.000038 ) 0.009371 0.009338 0.018685 ( 0.000047 0.000038 0.000082 ) unit cell: 7.362(15) 7.340(16) 7.349(19) 119.9(2) 120.2(2) 90.00(17) V = 280(1) OTKP changes: 41 1 1 1 OTKP changes: 41 1 1 1 OTKP changes: 41 1 1 1 UB - matrix: 0.087715 -0.044830 0.015254 ( 0.000161 0.000095 0.000186 ) 0.063272 0.093357 0.026278 ( 0.000148 0.000088 0.000171 ) 0.047808 0.056930 0.133315 ( 0.000228 0.000135 0.000263 ) M - matrix: 0.013983 0.004696 0.009374 ( 0.000040 0.000024 0.000039 ) 0.004696 0.013966 0.009359 ( 0.000024 0.000024 0.000030 ) 0.009374 0.009359 0.018696 ( 0.000039 0.000030 0.000071 ) UB fit with 41 obs out of 41 (total:41,skipped:0) (100.00%) unit cell: 7.362(11) 7.363(11) 7.356(15) 120.06(19) 120.11(19) 90.02(12) V = 281.2(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - -32.000,17 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 378 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 41 obs out of 41 (total:41,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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=17, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=17, start=1, end=17, Data range for background initialization of run 2 more narrow than requested (is:17,should:25) BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb 0 of 39 peaks identified as outliers and rejected 39 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 39 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 39 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 2.60 | 4 | 0.903 ( 0.087) | 0.919 ( 0.125) | 0.787 ( 0.151) | 2.38- 2.11 | 4 | 0.938 ( 0.087) | 0.946 ( 0.081) | 0.894 ( 0.317) | 1.84- 1.64 | 4 | 0.902 ( 0.064) | 0.929 ( 0.092) | 0.688 ( 0.244) | 1.57- 1.35 | 4 | 0.982 ( 0.033) | 0.998 ( 0.069) | 0.826 ( 0.140) | 1.35- 1.16 | 4 | 0.975 ( 0.050) | 1.039 ( 0.070) | 0.899 ( 0.206) | 1.14- 1.09 | 4 | 0.871 ( 0.044) | 0.941 ( 0.073) | 0.993 ( 0.606) | 1.00- 0.92 | 4 | 0.966 ( 0.046) | 0.972 ( 0.077) | 0.972 ( 0.313) | 0.89- 0.88 | 4 | 0.983 ( 0.032) | 0.931 ( 0.105) | 1.236 ( 0.468) | 0.88- 0.73 | 4 | 0.909 ( 0.045) | 0.908 ( 0.057) | 0.978 ( 0.343) | 0.72- 0.68 | 3 | 0.939 ( 0.032) | 0.936 ( 0.099) | 1.228 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 0.68 | 39 | 0.937 ( 0.068) | 0.952 ( 0.095) | 0.943 ( 0.389) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.0 | 25 | 0.976 ( 0.039) | 1.048 ( 0.061) | 1.083 ( 0.444) | 12.2-16.3 | 25 | 1.068 ( 0.399) | 1.086 ( 0.107) | 1.460 ( 1.999) | 16.5-20.6 | 25 | 0.942 ( 0.066) | 1.014 ( 0.097) | 1.032 ( 0.551) | 20.6-24.3 | 25 | 0.956 ( 0.058) | 1.015 ( 0.093) | 0.955 ( 0.408) | 24.5-27.6 | 25 | 0.954 ( 0.074) | 1.016 ( 0.117) | 1.063 ( 0.490) | 28.4-32.2 | 25 | 0.899 ( 0.088) | 0.911 ( 0.107) | 0.856 ( 0.416) | 32.4-36.3 | 25 | 0.954 ( 0.271) | 0.914 ( 0.131) | 1.156 ( 0.946) | 36.3-38.6 | 25 | 0.847 ( 0.096) | 0.807 ( 0.129) | 1.030 ( 0.536) | 38.6-41.3 | 25 | 0.890 ( 0.092) | 0.864 ( 0.160) | 1.046 ( 0.449) | 41.3-49.8 | 27 | 0.894 ( 0.103) | 0.806 ( 0.107) | 1.040 ( 0.528) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 252 | 0.938 ( 0.177) | 0.947 ( 0.149) | 1.072 ( 0.832) | Fitted profile normalization line parameters e1 dimension: a=-0.0036 b=1.14 e2 dimension: a=-0.0086 b=1.31 e3 dimension: a=0.0022 b=1.01 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5383 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 382671 Maximum peak integral for reflections I/sig<= 10000 - raw: 9635797 lp-corr: 1337669 PROFFITPEAK - Finished at Wed Aug 21 12:25:50 2019 PROFFITMAIN - Started at Wed Aug 21 12:25:50 2019 OTKP changes: 212 2 1 2 OTKP changes: 212 2 1 2 OTKP changes: 212 2 1 2 UB - matrix: 0.087498 -0.046029 0.017275 ( 0.000099 0.000064 0.000095 ) 0.064513 0.092365 0.027136 ( 0.000089 0.000058 0.000086 ) 0.045769 0.057886 0.132185 ( 0.000103 0.000067 0.000099 ) M - matrix: 0.013913 0.004581 0.009312 ( 0.000023 0.000013 0.000018 ) 0.004581 0.014001 0.009363 ( 0.000013 0.000014 0.000014 ) 0.009312 0.009363 0.018508 ( 0.000018 0.000014 0.000027 ) UB fit with 219 obs out of 252 (total:252,skipped:0) (86.90%) unit cell: 7.385(7) 7.370(6) 7.435(7) 120.56(9) 120.45(9) 89.19(7) V = 283.7(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 204 obs out of 213 (total:213,skipped:0) (95.77%) UB - matrix: 0.087505 -0.046049 0.017377 ( 0.000101 0.000063 0.000094 ) 0.064697 0.092371 0.027176 ( 0.000086 0.000054 0.000080 ) 0.045833 0.057931 0.132261 ( 0.000103 0.000065 0.000097 ) M - matrix: 0.013943 0.004602 0.009341 ( 0.000023 0.000013 0.000018 ) 0.004602 0.014009 0.009372 ( 0.000013 0.000014 0.000014 ) 0.009341 0.009372 0.018534 ( 0.000018 0.000014 0.000026 ) unit cell: 7.381(7) 7.368(6) 7.432(6) 120.53(9) 120.47(9) 89.25(7) V = 283.3(4) OTKP changes: 204 1 1 1 OTKP changes: 204 1 1 1 OTKP changes: 204 1 1 1 UB - matrix: 0.087442 -0.045998 0.017405 ( 0.000100 0.000063 0.000094 ) 0.064621 0.092321 0.027196 ( 0.000088 0.000055 0.000082 ) 0.045689 0.057855 0.132154 ( 0.000104 0.000065 0.000097 ) M - matrix: 0.013909 0.004587 0.009317 ( 0.000023 0.000013 0.000018 ) 0.004587 0.013986 0.009356 ( 0.000013 0.000014 0.000014 ) 0.009317 0.009356 0.018507 ( 0.000018 0.000014 0.000026 ) UB fit with 203 obs out of 213 (total:213,skipped:0) (95.31%) unit cell: 7.388(7) 7.373(6) 7.435(6) 120.53(9) 120.46(9) 89.24(7) V = 284.0(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.046) HKL list info: 1293 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087442 -0.045998 0.017405 ( 0.000100 0.000063 0.000094 ) 0.064620 0.092321 0.027196 ( 0.000088 0.000055 0.000082 ) 0.045688 0.057855 0.132154 ( 0.000104 0.000065 0.000097 ) M - matrix: 0.013909 0.004587 0.009317 ( 0.000023 0.000013 0.000018 ) 0.004587 0.013986 0.009356 ( 0.000013 0.000014 0.000014 ) 0.009317 0.009356 0.018507 ( 0.000018 0.000014 0.000026 ) UB fit with 203 obs out of 213 (total:213,skipped:0) (95.31%) unit cell: 7.388(7) 7.373(6) 7.435(6) 120.53(9) 120.46(9) 89.24(7) V = 284.0(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 213 (total:213,skipped:0) (97.18%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118147 0.039081 0.078860 ( 0.000077 0.000048 0.000071 ) 0.000072 0.111579 0.056267 ( 0.000074 0.000047 0.000069 ) 0.000017 -0.000041 0.095533 ( 0.000092 0.000058 0.000086 ) M - matrix: 0.013959 0.004625 0.009323 ( 0.000018 0.000011 0.000014 ) 0.004625 0.013977 0.009356 ( 0.000011 0.000011 0.000011 ) 0.009323 0.009356 0.018511 ( 0.000014 0.000011 0.000021 ) UB fit with 209 obs out of 213 (total:213,skipped:0) (98.12%) unit cell: 7.370(5) 7.376(5) 7.424(8) 120.45(9) 120.31(9) 89.46(6) V = 283.4(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 39 obs out of 39 (total:39,skipped:0) (100.00%) UB - matrix: 0.087764 -0.044791 0.015329 ( 0.000181 0.000105 0.000204 ) 0.063193 0.093307 0.026152 ( 0.000160 0.000092 0.000181 ) 0.047971 0.057033 0.133521 ( 0.000237 0.000137 0.000269 ) M - matrix: 0.013997 0.004701 0.009403 ( 0.000044 0.000025 0.000041 ) 0.004701 0.013965 0.009369 ( 0.000025 0.000025 0.000031 ) 0.009403 0.009369 0.018747 ( 0.000041 0.000031 0.000073 ) unit cell: 7.363(12) 7.362(12) 7.349(16) 120.0(2) 120.2(2) 90.01(13) V = 280.8(9) OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 Run 2 Omega scan: (-49.000 - -32.000,17 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 359 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.087764 -0.044791 0.015329 ( 0.000181 0.000105 0.000204 ) 0.063193 0.093307 0.026152 ( 0.000160 0.000092 0.000181 ) 0.047971 0.057033 0.133521 ( 0.000237 0.000137 0.000269 ) M - matrix: 0.013997 0.004701 0.009403 ( 0.000044 0.000025 0.000041 ) 0.004701 0.013965 0.009369 ( 0.000025 0.000025 0.000031 ) 0.009403 0.009369 0.018747 ( 0.000041 0.000031 0.000073 ) UB fit with 39 obs out of 39 (total:39,skipped:0) (100.00%) unit cell: 7.363(12) 7.362(12) 7.349(16) 120.0(2) 120.2(2) 90.01(13) V = 280.8(9) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=17, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=17, start=1, end=17, Data range for background initialization of run 2 more narrow than requested (is:17,should:25) BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.118002 0.039126 0.078735 ( 0.000073 0.000046 0.000070 ) 0.000006 0.111552 0.056236 ( 0.000071 0.000044 0.000068 ) -0.000024 -0.000098 0.095630 ( 0.000085 0.000053 0.000082 ) M - matrix: 0.013925 0.004618 0.009289 ( 0.000017 0.000010 0.000014 ) 0.004618 0.013975 0.009344 ( 0.000010 0.000011 0.000011 ) 0.009289 0.009344 0.018507 ( 0.000014 0.000011 0.000021 ) UB fit with 248 obs out of 252 (total:252,skipped:0) (98.41%) unit cell: 7.370(5) 7.373(4) 7.412(7) 120.41(8) 120.20(9) 89.55(5) V = 283.3(4) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 43 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof 1180 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:25:52 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.046) Run 2 Omega scan: (-49.000 - -32.000,17 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-529.0000 max=8347617.0000 PROFFIT INFO: signal sum lp corr: min=-629.9519 max=1164036.6594 PROFFIT INFO: background sum: min=100.0000 max=14500.0000 PROFFIT INFO: background sum sig2: min=421.0000 max=4889.0000 PROFFIT INFO: num of signal pixels: min=41 max=488 PROFFIT INFO: Inet: min=-1007.9230 max=1862458.6250 PROFFIT INFO: sig(Inet): min=63.4244 max=22450.0098 PROFFIT INFO: Inet/sig(Inet): min=-1.52 max=172.37 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 136 451 657 755 811 927 995 1047 1125 1173 1180 Percent 11.5 38.2 55.7 64.0 68.7 78.6 84.3 88.7 95.3 99.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1180 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 1180 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1862459- 109629 118 378620.70 72.35 100.00 107758- 4099 118 24825.57 18.70 100.00 4080- 1961 118 2694.27 6.52 97.46 1951- 1115 118 1445.78 3.51 41.53 1111- 722 118 895.72 2.03 12.71 718- 450 118 586.63 1.52 6.78 449- 254 118 357.23 1.02 1.69 254- 98 118 170.22 0.46 0.00 94- -21 118 36.56 0.16 0.00 -22- -1008 118 -200.86 -0.39 0.00 ------------------------------------------------------------------------------------ 1862459- -1008 1180 40943.18 10.59 36.02 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.03- 1.64 118 100335.86 14.18 66.95 1.64- 1.26 118 74962.86 18.46 51.69 1.23- 1.05 118 68968.85 20.49 70.34 1.05- 0.95 118 37807.61 11.40 22.03 0.95- 0.88 118 42200.59 12.47 48.31 0.88- 0.80 118 22846.43 7.67 29.66 0.80- 0.74 118 16540.10 5.51 23.73 0.74- 0.71 118 23124.86 7.46 17.80 0.71- 0.67 118 20283.62 6.83 23.73 0.67- 0.62 118 2361.04 1.42 5.93 ------------------------------------------------------------------------------------ 6.03- 0.62 1180 40943.18 10.59 36.02 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:25:52 2019 Sorting 1180 observations 37 unique observations with > 7.00 F2/sig(F2) 1180 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 16 120 Total number of frames 120 Maximum number of 37 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1180 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 4 31 Total number of frames 31 271 observations > 7.00 F2/sig(F2) 271 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 4 31 Total number of frames 31 Removing 'redundancy=1' reflections Average redundancy: 2.1 (Out of 271 removed 202 = 69, unique = 33) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 1bar 69 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 4 31 Total number of frames 31 Frame #12 of 31 skipped from refinement Frame #17 of 31 skipped from refinement Frame #20 of 31 skipped from refinement Frame #24 of 31 skipped from refinement 4 frames need to be skipped from refinement, because of missing redundant and/or observable data 33 unique data precomputed (should be 33) 33 unique data with 69 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.1 (Out of 69 removed 0 = 69, unique = 33) 33 unique data precomputed (should be 33) 33 unique data with 69 observations RMS deviation of equivalent data = 0.30949 Rint = 0.30227 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.30227, wR= 0.33606 Trying model 1 (ne=2, no=0)... Results: Rint= 0.10251, wR= 0.09050, Acormin=0.231, Acormax=1.579, Acor_av=0.863 F test: Probability=1.000, F= 7.487 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04656, wR= 0.05725, Acormin=0.078, Acormax=1.463, Acor_av=0.640 F test: Probability=1.000, F= 4.379 Final absorption model (ne=2, no=1): Rint= 0.04656, Acormin=0.078, Acormax=1.463, Acor_av=0.640 Combined refinement in use Rint: 0.30343 There are 27 active scales (one needs to be fixed) Refinement control: frame scale #29 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 1 (8 parameters) Refinement control: 34 pars with 595 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30949 Using Levenberg-Marquardt: 0.00010 New wR= 0.21232 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.30227 with corrections 0.21983 Rint for all data: 0.30343 with corrections 0.22083 0 observations identified as outliers and rejected Cycle 2 wR= 0.21232 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= 0.03527 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.30227 with corrections 0.02528 Rint for all data: 0.30343 with corrections 0.02713 0 observations identified as outliers and rejected Cycle 3 wR= 0.03527 Using Levenberg-Marquardt: 0.01000 New wR= 0.02757 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.30227 with corrections 0.02002 Rint for all data: 0.30343 with corrections 0.02191 0 observations identified as outliers and rejected Cycle 4 wR= 0.02757 Using Levenberg-Marquardt: 0.00100 New wR= 0.34933 Using Levenberg-Marquardt: 0.01000 New wR= 0.02701 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.30227 with corrections 0.01923 Rint for all data: 0.30343 with corrections 0.02111 0 observations identified as outliers and rejected Cycle 5 wR= 0.02701 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.02687 There are 4 clusters with unrefined scales (size 1-1) Rint for refined data: 0.30227 with corrections 0.01954 Rint for all data: 0.30343 with corrections 0.02142 0 observations identified as outliers and rejected Final wR= 0.02687 Final frame scales: Min= 0.4099 Max= 1.0290 Final absorption correction factors: Amin= 0.4639 Amax= 1.6716 PROFFIT INFO: Inet (after scale3 abspack): min=-899.8885 max=1251710.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=55.8634 max=25500.8125 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 0, Friedel: 1 Min/max for: run:1/2 frame:1/103 1180 reflections read from tmp file 896 reflections are rejected (3 as outliers, 893 as groups of 1 refl) Redundancy: 1 2 3+ Number of groups: 0 136 4 Initial Chi^2= 0.67541 Cycle 1, Chi^2= 0.92154 Current error model SIG(F2)^2 = 78.59*I_RAW + 14.74*I_BACK+(0.03667*)^2 Cycle 2, Chi^2= 1.03467 Current error model SIG(F2)^2 = 95.91*I_RAW + 7.40*I_BACK+(0.02092*)^2 Cycle 3, Chi^2= 1.01072 Current error model SIG(F2)^2 = 97.98*I_RAW + 5.73*I_BACK+(0.02843*)^2 Cycle 4, Chi^2= 1.01575 Current error model SIG(F2)^2 = 107.89*I_RAW + 4.09*I_BACK+(0.02330*)^2 Cycle 5, Chi^2= 1.00528 Current error model SIG(F2)^2 = 108.97*I_RAW + 3.45*I_BACK+(0.02697*)^2 Cycle 6, Chi^2= 1.00782 Current error model SIG(F2)^2 = 113.83*I_RAW + 2.79*I_BACK+(0.02432*)^2 Cycle 7, Chi^2= 1.00254 Current error model SIG(F2)^2 = 114.21*I_RAW + 2.52*I_BACK+(0.02633*)^2 Cycle 8, Chi^2= 1.00395 Current error model SIG(F2)^2 = 116.72*I_RAW + 2.22*I_BACK+(0.02484*)^2 Cycle 9, Chi^2= 1.00115 Current error model SIG(F2)^2 = 116.78*I_RAW + 2.10*I_BACK+(0.02599*)^2 Cycle 10, Chi^2= 1.00202 Current error model SIG(F2)^2 = 118.10*I_RAW + 1.96*I_BACK+(0.02512*)^2 Final Chi^2= 1.00202 Final error model SIG(F2)^2 = 118.10*I_RAW + 1.96*I_BACK+(0.02512*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1251710- 94663 118 368259.17 28.85 100.00 94600- 3869 118 22438.60 11.36 100.00 3706- 1932 118 2641.38 5.00 93.22 1903- 1032 118 1370.79 3.16 40.68 1032- 685 118 829.74 2.35 17.80 675- 432 118 535.82 1.89 5.08 430- 246 118 335.99 1.65 3.39 245- 94 118 160.61 1.10 0.85 93- -19 118 36.75 0.42 0.00 -19- -900 118 -189.98 -0.80 0.00 ------------------------------------------------------------------------------------ 1251710- -900 1180 39641.89 5.50 36.10 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.03- 1.64 118 99640.24 9.01 67.80 1.64- 1.26 118 78888.54 8.14 50.85 1.23- 1.05 118 69963.25 8.68 72.03 1.05- 0.95 118 34270.95 4.89 22.88 0.95- 0.88 118 35391.87 6.55 48.31 0.88- 0.80 118 24111.77 4.28 28.81 0.80- 0.74 118 15140.75 3.47 22.88 0.74- 0.71 118 19621.39 4.54 17.80 0.71- 0.67 118 17462.83 4.02 23.73 0.67- 0.62 118 1927.28 1.37 5.93 ------------------------------------------------------------------------------------ 6.03- 0.62 1180 39641.89 5.50 36.10 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.03- 1.64 118 99640.24 9.01 67.80 6.03- 1.26 236 89264.39 8.57 59.32 6.03- 1.05 354 82830.68 8.61 63.56 6.03- 0.95 472 70690.75 7.68 53.39 6.03- 0.88 590 63630.97 7.45 52.37 6.03- 0.80 708 57044.44 6.93 48.45 6.03- 0.74 826 51058.20 6.43 44.79 6.03- 0.71 944 47128.59 6.20 41.42 6.03- 0.67 1062 43832.40 5.95 39.45 6.03- 0.62 1180 39641.89 5.50 36.10 ------------------------------------------------------------------------------------ 6.03- 0.62 1180 39641.89 5.50 36.10 Scale applied to data: s=0.798906 (maximum obs:1251710.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.021; Rsigma 0.040: data 1180 -> merged 1033 With outlier rejection... Rint 0.021; Rsigma 0.040: data 1179 -> merged 1033 Rejected total: 1, method kkm 1, method Blessing 0 Completeness direct cell (a, b, c) = (7.370, 7.373, 7.412), (alpha, beta, gamma) = (120.406, 120.200, 89.551) wavelength: 0.709300 dmin, dmax value (Ang): 0.624717, 6.039580 completeness table (Laue group: P1, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.39 128 215 1.33 59.53 170 1.39 - 1.13 130 215 1.12 60.47 146 1.13 - 0.97 112 215 1.12 52.09 125 0.97 - 0.88 108 215 1.11 50.23 120 0.88 - 0.82 96 215 1.13 44.65 108 0.82 - 0.78 89 215 1.13 41.40 101 0.78 - 0.73 90 215 1.09 41.86 98 0.73 - 0.70 87 215 1.11 40.47 97 0.70 - 0.67 70 215 1.11 32.56 78 0.67 - 0.65 77 216 1.16 35.65 89 --------------------------------------------------------------- 7.36 - 0.65 987 2151 1.15 45.89 1132 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:25:52 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.370329 7.372612 7.412369 120.4058 120.1995 89.5509 1179 Reflections read from file xs2212a.hkl 1168 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 5.52 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 583 581 584 583 874 784 789 1168 N (int>3sigma) = 0 145 156 215 146 258 302 309 423 Mean intensity = 0.0 0.9 1.0 1.4 0.9 1.1 30.9 35.2 32.0 Mean int/sigma = 0.0 2.4 2.5 3.3 2.3 2.7 5.6 5.8 5.5 Lattice type: P chosen Volume: 283.31 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 Unitcell: 7.347 7.362 7.369 60.06 89.76 60.14 Niggli form: a.a = 53.981 b.b = 54.194 c.c = 54.304 b.c = 27.071 a.c = 0.230 a.b = 26.927 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.920 CUBIC F-lattice R(int) = 0.170 [ 946] Vol = 1133.2 Cell: 10.428 10.466 10.384 89.98 89.83 89.61 Volume: 1133.23 Matrix: 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.371 RHOMBOHEDRAL R-lattice R(int) = 0.133 [ 599] Vol = 849.9 Cell: 7.370 7.347 18.119 89.65 90.46 119.97 Volume: 849.92 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 -1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.371 RHOMBOHEDRAL R-lattice R(int) = 0.112 [ 160] Vol = 849.9 Trigonal Cell: 7.370 7.347 18.119 89.65 90.46 119.97 Volume: 849.92 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 -1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.625 ORTHORHOMBIC I-lattice R(int) = 0.090 [ 587] Vol = 566.6 Cell: 7.370 10.428 7.373 89.60 89.55 89.84 Volume: 566.61 Matrix: 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.476 MONOCLINIC I-lattice R(int) = 0.064 [ 449] Vol = 566.6 Cell: 7.373 7.370 10.428 89.84 90.40 90.45 Volume: 566.61 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.239 MONOCLINIC I-lattice R(int) = 0.130 [ 432] Vol = 566.6 Cell: 7.369 7.347 10.466 89.73 90.29 90.24 Volume: 566.61 Matrix: 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.021 [ 146] Vol = 283.3 Cell: 7.347 7.362 7.369 60.06 89.76 60.14 Volume: 283.31 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 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 0 584 0 781 784 1168 N (int>3sigma) = 0 0 0 0 215 0 310 306 423 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.9 33.3 32.0 Mean int/sigma = 0.0 0.0 0.0 0.0 3.3 0.0 5.6 5.7 5.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.252 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 98 208 N I>3s 1 1 1 101 0.1 0.1 -0.0 2.1 1.5 1.5 0.2 4.5 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 0.170 873 Fd-3m 1 1 227 C N N N N 37 2284 0.170 934 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.428101 10.465610 10.383897 89.9823 89.8290 89.6066 ZERR 1.00 0.021787 0.002046 0.011679 0.0057 0.0013 0.2251 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1251710- 96847 117 117 103 1.1 370597.60 28.93 0.018 0.019 94663- 3706 121 120 103 1.2 22838.60 11.33 0.035 0.035 3697- 1902 119 119 103 1.2 2600.54 4.91 0.082 0.084 1890- 1027 116 116 103 1.1 1345.49 3.16 0.153 0.152 1024- 675 114 114 103 1.1 835.10 2.31 0.154 0.154 675- 438 119 119 103 1.2 542.03 1.92 0.179 0.179 438- 245 115 115 103 1.1 339.66 1.65 0.277 0.277 238- 97 122 122 103 1.2 168.40 1.09 0.475 0.493 96- -17 121 121 103 1.2 37.17 0.42 0.798 1.444 -17- -900 116 116 106 1.1 -186.14 -0.75 0.834 1.009 ------------------------------------------------------------------------------------------- 1251710- -900 1180 1179 1033 1.1 39667.77 5.49 0.021 0.022 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-1.46 143 142 103 1.4 140453.64 11.52 0.024 0.026 0.029 1.46-1.20 115 115 103 1.1 10177.26 4.28 0.067 0.067 0.058 1.20-1.04 116 116 103 1.1 70780.28 8.06 0.011 0.011 0.034 1.04-0.94 114 114 103 1.1 35503.32 5.17 0.007 0.007 0.038 0.94-0.86 117 117 103 1.1 50098.99 8.08 0.012 0.012 0.043 0.86-0.80 116 116 103 1.1 9943.11 2.74 0.147 0.148 0.067 0.80-0.74 112 112 103 1.1 15909.70 3.54 0.020 0.020 0.062 0.74-0.71 116 116 103 1.1 19973.27 4.57 0.026 0.026 0.061 0.71-0.67 115 115 103 1.1 17868.76 4.09 0.032 0.032 0.070 0.67-0.62 116 116 106 1.1 1956.37 1.39 0.420 0.447 0.204 ------------------------------------------------------------------------------------------------------ inf-0.62 1180 1179 1033 1.1 39667.77 5.49 0.021 0.022 0.040 inf-0.66 1133 1132 987 1.1 41141.04 5.65 0.021 0.022 0.039 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-1.46 142 175 103 58.9 1.4 140453.64 13.91 0.024 0.020 1.46-1.20 115 166 103 62.0 1.1 10177.26 4.49 0.067 0.130 1.20-1.04 116 189 103 54.5 1.1 70780.28 8.73 0.011 0.023 1.04-0.94 114 194 103 53.1 1.1 35503.32 5.47 0.007 0.027 0.94-0.86 117 218 103 47.2 1.1 50098.99 9.08 0.012 0.028 0.86-0.80 116 231 103 44.6 1.1 9943.11 2.86 0.147 0.255 0.80-0.74 112 245 103 42.0 1.1 15909.70 3.78 0.020 0.041 0.74-0.71 116 259 103 39.8 1.1 19973.27 5.09 0.026 0.041 0.71-0.67 115 304 103 33.9 1.1 17868.76 4.37 0.032 0.049 0.67-0.62 116 474 106 22.4 1.1 1956.37 1.47 0.420 0.470 -------------------------------------------------------------------------------------------- inf-0.62 1179 2459 1033 42.0 1.1 39667.77 6.11 0.021 0.025 inf-0.66 1132 2139 987 46.1 1.1 41141.04 6.30 0.021 0.025 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 2.0 -1.0 -1.0 0.0 1.0 -1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 2.0 -1.0 -1.0 0.0 1.0 -1.0 0.0 No constraint UB - matrix: 0.008570 -0.012439 0.066614 ( 0.000028 0.000034 0.000028 ) 0.013447 -0.065134 -0.013917 ( 0.000029 0.000034 0.000028 ) 0.066099 0.014302 -0.005953 ( 0.000038 0.000045 0.000037 ) M - matrix: 0.004623 -0.000037 -0.000010 ( 0.000005 0.000004 0.000003 ) -0.000037 0.004602 -0.000007 ( 0.000004 0.000005 0.000003 ) -0.000010 -0.000007 0.004667 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: 0.008570 -0.012439 0.066614 ( 0.000028 0.000034 0.000028 ) 0.013447 -0.065134 -0.013917 ( 0.000029 0.000034 0.000028 ) 0.066099 0.014302 -0.005953 ( 0.000038 0.000045 0.000037 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) unit cell: 10.432(5) 10.457(6) 10.383(4) 89.91(4) 89.88(4) 89.54(4) V = 1132.6(10) unit cell: 10.4237(11) 10.4237(11) 10.4237(11) 90.0 90.0 90.0 V = 1132.6(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.046) Run 2 Omega scan: (-49.000 - -32.000,17 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-529.0000 max=8347617.0000 PROFFIT INFO: signal sum lp corr: min=-629.9519 max=1164036.6594 PROFFIT INFO: background sum: min=100.0000 max=14500.0000 PROFFIT INFO: background sum sig2: min=421.0000 max=4889.0000 PROFFIT INFO: num of signal pixels: min=41 max=488 PROFFIT INFO: Inet: min=-1007.9230 max=1862458.6250 PROFFIT INFO: sig(Inet): min=63.4244 max=22450.0098 PROFFIT INFO: Inet/sig(Inet): min=-1.52 max=172.37 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 272 902 1314 1510 1622 1854 1990 2094 2250 2346 2360 Percent 11.5 38.2 55.7 64.0 68.7 78.6 84.3 88.7 95.3 99.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1180 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 1180 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1862459- 109629 118 378620.70 72.35 100.00 107758- 4099 118 24825.57 18.70 100.00 4080- 1961 118 2694.27 6.52 97.46 1951- 1115 118 1445.78 3.51 41.53 1111- 722 118 895.72 2.03 12.71 718- 450 118 586.63 1.52 6.78 449- 254 118 357.23 1.02 1.69 254- 98 118 170.22 0.46 0.00 94- -21 118 36.56 0.16 0.00 -22- -1008 118 -200.86 -0.39 0.00 ------------------------------------------------------------------------------------ 1862459- -1008 1180 40943.18 10.59 36.02 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.64 118 100355.38 14.21 66.95 1.64- 1.26 118 74943.33 18.43 51.69 1.23- 1.05 118 68968.85 20.49 70.34 1.05- 0.95 118 37822.07 11.41 22.03 0.95- 0.88 118 42186.01 12.43 48.31 0.88- 0.80 118 22843.54 7.68 29.66 0.80- 0.74 118 16551.14 5.54 23.73 0.74- 0.71 118 23138.72 7.47 18.64 0.71- 0.67 118 20300.98 6.86 22.88 0.67- 0.63 118 2321.79 1.37 5.93 ------------------------------------------------------------------------------------ 6.01- 0.63 1180 40943.18 10.59 36.02 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:25:53 2019 Sorting 1180 observations 37 unique observations with > 7.00 F2/sig(F2) 1180 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 16 120 Total number of frames 120 Maximum number of 37 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1180 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 4 31 Total number of frames 31 271 observations > 7.00 F2/sig(F2) 271 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 4 31 Total number of frames 31 Removing 'redundancy=1' reflections Average redundancy: 6.6 (Out of 271 removed 8 = 263, unique = 40) 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 263 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 4 31 Total number of frames 31 40 unique data precomputed (should be 40) 40 unique data with 263 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.6 (Out of 263 removed 0 = 263, unique = 40) 40 unique data precomputed (should be 40) 40 unique data with 263 observations RMS deviation of equivalent data = 0.30745 Rint = 0.25825 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.25181, wR= 0.34944 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13479, wR= 0.24492, Acormin=0.420, Acormax=1.317, Acor_av=0.862 F test: Probability=1.000, F= 3.411 Trying model 2 (ne=2, no=1)... Results: Rint= 0.16174, wR= 0.24624, Acormin=0.190, Acormax=1.172, Acor_av=0.632 F test: Probability=0.000, F= 0.685 Final absorption model (ne=2, no=0): Rint= 0.13479, Acormin=0.420, Acormax=1.317, Acor_av=0.862 Combined refinement in use Rint: 0.26002 There are 31 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 35 pars with 630 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30745 Using Levenberg-Marquardt: 0.00010 New wR= 0.16756 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25825 with corrections 0.13347 Rint for all data: 0.26002 with corrections 0.13658 0 observations identified as outliers and rejected Cycle 2 wR= 0.16756 Using Levenberg-Marquardt: 0.00001 New wR= 0.16232 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25825 with corrections 0.13173 Rint for all data: 0.26002 with corrections 0.13483 0 observations identified as outliers and rejected Cycle 3 wR= 0.16232 Using Levenberg-Marquardt: 0.00000 New wR= 0.16054 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25825 with corrections 0.13695 Rint for all data: 0.26002 with corrections 0.14003 0 observations identified as outliers and rejected Cycle 4 wR= 0.16054 Using Levenberg-Marquardt: 0.00000 New wR= 0.16169 Using Levenberg-Marquardt: 0.00000 New wR= 0.16169 Using Levenberg-Marquardt: 0.00001 New wR= 0.16169 Using Levenberg-Marquardt: 0.00010 New wR= 0.16169 Using Levenberg-Marquardt: 0.00100 New wR= 0.16168 Using Levenberg-Marquardt: 0.01000 New wR= 0.16161 Using Levenberg-Marquardt: 0.10000 New wR= 0.16127 Using Levenberg-Marquardt: 1.00000 New wR= 0.16082 Using Levenberg-Marquardt: 10.00000 New wR= 0.16059 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25825 with corrections 0.13698 Rint for all data: 0.26002 with corrections 0.14005 Final wR= 0.16059 Final frame scales: Min= 0.3947 Max= 1.0562 Final absorption correction factors: Amin= 0.6458 Amax= 1.3273 PROFFIT INFO: Inet (after scale3 abspack): min=-1062.3115 max=1169134.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=48.1873 max=24544.1094 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/103 1180 reflections read from tmp file 112 reflections are rejected (97 as outliers, 15 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 12 12 15 11 11 11 13 9 43 Initial Chi^2= 0.80053 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.00882 Current error model SIG(F2)^2 = 142.36*I_RAW + 0.00*I_BACK+(0.04302*)^2 Cycle 2, Chi^2= 1.00245 Current error model SIG(F2)^2 = 148.32*I_RAW + 0.00*I_BACK+(0.03455*)^2 Cycle 3, Chi^2= 1.00017 Current error model SIG(F2)^2 = 149.37*I_RAW + 0.00*I_BACK+(0.03346*)^2 Cycle 4, Chi^2= 1.00003 Current error model SIG(F2)^2 = 149.54*I_RAW + 0.00*I_BACK+(0.03323*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 149.57*I_RAW + 0.00*I_BACK+(0.03318*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 149.57*I_RAW + 0.00*I_BACK+(0.03318*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1169134- 105864 118 343470.53 23.93 100.00 105414- 3716 118 24796.58 9.71 100.00 3662- 1803 118 2572.34 4.47 88.98 1761- 1043 118 1354.88 2.83 24.58 1038- 708 118 857.13 2.01 5.93 706- 449 118 578.85 1.76 3.39 448- 246 118 342.13 1.54 3.39 244- 94 118 165.73 1.10 2.54 91- -21 118 35.95 1.97 1.69 -22- -1062 118 -189.33 -0.81 0.00 ------------------------------------------------------------------------------------ 1169134- -1062 1180 37398.48 4.85 33.05 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.64 118 86324.38 7.66 64.41 1.64- 1.26 118 67685.05 8.40 49.15 1.23- 1.05 118 68179.17 7.28 67.80 1.05- 0.95 118 34200.41 4.18 22.88 0.95- 0.88 118 36027.09 5.55 40.68 0.88- 0.80 118 24512.48 3.70 24.58 0.80- 0.74 118 15504.16 3.06 17.80 0.74- 0.71 118 19508.12 3.95 16.10 0.71- 0.67 118 19487.86 3.59 22.88 0.67- 0.63 118 2556.05 1.16 4.24 ------------------------------------------------------------------------------------ 6.01- 0.63 1180 37398.48 4.85 33.05 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.01- 1.64 118 86324.38 7.66 64.41 6.01- 1.26 236 77004.71 8.03 56.78 6.01- 1.05 354 74062.87 7.78 60.45 6.01- 0.95 472 64097.25 6.88 51.06 6.01- 0.88 590 58483.22 6.61 48.98 6.01- 0.80 708 52821.43 6.13 44.92 6.01- 0.74 826 47490.39 5.69 41.04 6.01- 0.71 944 43992.61 5.47 37.92 6.01- 0.67 1062 41269.86 5.26 36.25 6.01- 0.63 1180 37398.48 4.85 33.05 ------------------------------------------------------------------------------------ 6.01- 0.63 1180 37398.48 4.85 33.05 Scale applied to data: s=0.855333 (maximum obs:1169134.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.140; Rsigma 0.049: data 1180 -> merged 155 With outlier rejection... Rint 0.095; Rsigma 0.049: data 1155 -> merged 155 Rejected total: 25, method kkm 24, method Blessing 1 Completeness direct cell (a, b, c) = (10.424, 10.424, 10.424), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627434, 6.018139 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.76 14 14 7.00 100.00 98 1.74 - 1.27 14 14 8.21 100.00 115 1.26 - 1.06 14 14 9.43 100.00 132 1.05 - 0.97 14 14 8.00 100.00 112 0.95 - 0.88 14 14 8.93 100.00 125 0.87 - 0.81 14 14 7.36 100.00 103 0.80 - 0.76 14 14 8.14 100.00 114 0.76 - 0.72 13 14 7.46 92.86 97 0.72 - 0.69 13 14 7.77 92.86 101 0.69 - 0.65 18 19 6.50 94.74 117 --------------------------------------------------------------- 7.36 - 0.65 142 145 7.85 97.93 1114 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:25:52 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.370329 7.372612 7.412369 120.4058 120.1995 89.5509 1179 Reflections read from file xs2212a.hkl 1168 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 5.52 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 583 581 584 583 874 784 789 1168 N (int>3sigma) = 0 145 156 215 146 258 302 309 423 Mean intensity = 0.0 0.9 1.0 1.4 0.9 1.1 30.9 35.2 32.0 Mean int/sigma = 0.0 2.4 2.5 3.3 2.3 2.7 5.6 5.8 5.5 Lattice type: P chosen Volume: 283.31 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 Unitcell: 7.347 7.362 7.369 60.06 89.76 60.14 Niggli form: a.a = 53.981 b.b = 54.194 c.c = 54.304 b.c = 27.071 a.c = 0.230 a.b = 26.927 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.920 CUBIC F-lattice R(int) = 0.170 [ 946] Vol = 1133.2 Cell: 10.428 10.466 10.384 89.98 89.83 89.61 Volume: 1133.23 Matrix: 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.371 RHOMBOHEDRAL R-lattice R(int) = 0.133 [ 599] Vol = 849.9 Cell: 7.370 7.347 18.119 89.65 90.46 119.97 Volume: 849.92 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 -1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.371 RHOMBOHEDRAL R-lattice R(int) = 0.112 [ 160] Vol = 849.9 Trigonal Cell: 7.370 7.347 18.119 89.65 90.46 119.97 Volume: 849.92 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 -1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.625 ORTHORHOMBIC I-lattice R(int) = 0.090 [ 587] Vol = 566.6 Cell: 7.370 10.428 7.373 89.60 89.55 89.84 Volume: 566.61 Matrix: 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.476 MONOCLINIC I-lattice R(int) = 0.064 [ 449] Vol = 566.6 Cell: 7.373 7.370 10.428 89.84 90.40 90.45 Volume: 566.61 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.239 MONOCLINIC I-lattice R(int) = 0.130 [ 432] Vol = 566.6 Cell: 7.369 7.347 10.466 89.73 90.29 90.24 Volume: 566.61 Matrix: 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.021 [ 146] Vol = 283.3 Cell: 7.347 7.362 7.369 60.06 89.76 60.14 Volume: 283.31 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 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 0 584 0 781 784 1168 N (int>3sigma) = 0 0 0 0 215 0 310 306 423 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.9 33.3 32.0 Mean int/sigma = 0.0 0.0 0.0 0.0 3.3 0.0 5.6 5.7 5.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.252 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 98 208 N I>3s 1 1 1 101 0.1 0.1 -0.0 2.1 1.5 1.5 0.2 4.5 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 0.170 873 Fd-3m 1 1 227 C N N N N 37 2284 0.170 934 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.428101 10.465610 10.383897 89.9823 89.8290 89.6066 ZERR 1.00 0.021787 0.002046 0.011679 0.0057 0.0013 0.2251 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1021852- 84658 141 124 25 5.0 301183.83 22.57 0.091 0.099 69906- 2096 206 202 25 8.1 5389.58 6.35 0.135 0.129 2083- 819 223 223 25 8.9 1117.23 2.39 0.282 0.341 804- 348 212 212 25 8.5 515.78 1.56 0.429 0.550 344- 53 184 184 25 7.4 218.52 1.11 0.590 0.831 50- -512 214 210 30 7.0 -18.78 0.05 0.913 2.464 ------------------------------------------------------------------------------------------- 1021852- -512 1180 1155 155 7.5 33619.26 4.47 0.095 0.103 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-1.36 207 201 25 8.0 73811.19 7.63 0.092 0.102 0.037 1.30-1.01 214 212 25 8.5 39375.33 4.63 0.106 0.116 0.045 1.00-0.85 216 211 26 8.1 41621.82 5.57 0.077 0.078 0.050 0.84-0.75 202 199 25 8.0 12645.46 2.74 0.115 0.120 0.074 0.74-0.68 187 186 25 7.4 17576.53 3.44 0.109 0.127 0.077 0.68-0.63 154 146 29 5.0 7388.64 1.95 0.120 0.102 0.108 ------------------------------------------------------------------------------------------------------ inf-0.63 1180 1155 155 7.5 33619.26 4.47 0.095 0.103 0.049 inf-0.66 1133 1112 141 7.9 34710.13 4.58 0.095 0.102 0.049 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-1.36 201 25 25 100.0 8.0 73811.19 20.85 0.092 0.020 1.30-1.01 212 25 25 100.0 8.5 39375.33 12.88 0.106 0.018 1.00-0.85 211 26 26 100.0 8.1 41621.82 16.96 0.077 0.024 0.84-0.75 199 25 25 100.0 8.0 12645.46 6.91 0.115 0.028 0.74-0.68 186 26 25 96.2 7.4 17576.53 9.76 0.109 0.030 0.68-0.63 146 34 29 85.3 5.0 7388.64 4.61 0.120 0.052 -------------------------------------------------------------------------------------------- inf-0.63 1155 162 155 95.7 7.5 33619.26 12.44 0.095 0.023 inf-0.66 1112 143 141 98.6 7.9 34710.13 12.83 0.095 0.022 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:28:00 2019) ID: 3668; threads 39; handles 810; mem 513924.00 (1196496.00)kB; time: 1w 4d 22h 38m 48s MEMORY INFO: Memory PF:71.0, Ph:524.0, V:1168.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:501.9,peak PF: 700.2, WS: 470.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:74.0, Ph:525.0, V:1170.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:503.7,peak PF: 700.2, WS: 472.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:28:00 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000105 0.000067 0.000101 ) 0.064809 0.092374 0.027273 ( 0.000091 0.000058 0.000087 ) 0.045523 0.057900 0.132205 ( 0.000102 0.000065 0.000098 ) 7.38096 ( 0.00695 ) 7.36649 ( 0.00667 ) 7.42630 ( 0.00659 ) 120.52449 ( 0.09469 ) 120.40327 ( 0.09627 ) 89.27095 ( 0.07489 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:28:00 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000105 0.000067 0.000101 ) 0.064809 0.092374 0.027273 ( 0.000091 0.000058 0.000087 ) 0.045523 0.057900 0.132205 ( 0.000102 0.000065 0.000098 ) M - matrix: 0.013914 0.004584 0.009286 ( 0.000024 0.000014 0.000018 ) 0.004584 0.013994 0.009346 ( 0.000014 0.000015 0.000014 ) 0.009286 0.009346 0.018464 ( 0.000018 0.000014 0.000026 ) unit cell: 7.381(7) 7.366(7) 7.426(7) 120.52(9) 120.40(10) 89.27(7) V = 283.3(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 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: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb PROFFITPEAK info: 153 peaks in the peak location table UB fit with 24 obs out of 85 (total:85,skipped:0) (28.24%) UB - matrix: 0.086211 -0.046825 0.015252 ( 0.001311 0.000653 0.001430 ) 0.062054 0.091632 0.025541 ( 0.000985 0.000490 0.001074 ) 0.045247 0.057518 0.132489 ( 0.001818 0.000905 0.001983 ) M - matrix: 0.013330 0.004252 0.008895 ( 0.000305 0.000169 0.000294 ) 0.004252 0.013897 0.009247 ( 0.000169 0.000150 0.000204 ) 0.008895 0.009247 0.018438 ( 0.000294 0.000204 0.000530 ) unit cell: 7.46(9) 7.37(8) 7.38(11) 121(1) 120(1) 88.7(9) V = 287(7) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 24 obs out of 85 (total:85,skipped:0) (28.24%) UB - matrix: 0.086211 -0.046825 0.015252 ( 0.001311 0.000653 0.001430 ) 0.062054 0.091632 0.025541 ( 0.000985 0.000490 0.001074 ) 0.045247 0.057518 0.132489 ( 0.001818 0.000905 0.001983 ) M - matrix: 0.013330 0.004252 0.008895 ( 0.000305 0.000169 0.000294 ) 0.004252 0.013897 0.009247 ( 0.000169 0.000150 0.000204 ) 0.008895 0.009247 0.018438 ( 0.000294 0.000204 0.000530 ) unit cell: 7.46(9) 7.37(8) 7.38(11) 121(1) 120(1) 88.7(9) V = 287(7) OTKP changes: 21 1 1 1 OTKP changes: 21 1 1 1 OTKP changes: 21 1 1 1 UB - matrix: 0.087747 -0.044923 0.015036 ( 0.000298 0.000196 0.000347 ) 0.062751 0.093151 0.025778 ( 0.000325 0.000213 0.000378 ) 0.048027 0.057113 0.133711 ( 0.000307 0.000201 0.000357 ) M - matrix: 0.013944 0.004646 0.009359 ( 0.000073 0.000044 0.000060 ) 0.004646 0.013957 0.009362 ( 0.000044 0.000049 0.000052 ) 0.009359 0.009362 0.018769 ( 0.000060 0.000052 0.000098 ) UB fit with 80 obs out of 85 (total:85,skipped:0) (94.12%) unit cell: 7.36(2) 7.36(2) 7.34(2) 120.1(3) 120.1(3) 89.9(2) V = 281(2) UB fit with 80 obs out of 85 (total:85,skipped:0) (94.12%) UB - matrix: 0.087747 -0.044923 0.015036 ( 0.000298 0.000196 0.000347 ) 0.062752 0.093151 0.025779 ( 0.000325 0.000213 0.000378 ) 0.048028 0.057113 0.133712 ( 0.000307 0.000201 0.000357 ) M - matrix: 0.013944 0.004647 0.009359 ( 0.000073 0.000044 0.000060 ) 0.004647 0.013957 0.009363 ( 0.000044 0.000049 0.000052 ) 0.009359 0.009363 0.018770 ( 0.000060 0.000052 0.000098 ) unit cell: 7.36(2) 7.36(2) 7.34(2) 120.1(3) 120.1(3) 89.9(2) V = 281(2) OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 85 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Run 2 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 456 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 80 obs out of 85 (total:85,skipped:0) (94.12%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb 0 of 64 peaks identified as outliers and rejected 64 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 64 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 64 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.39 | 6 | 0.891 ( 0.085) | 0.902 ( 0.107) | 0.770 ( 0.156) | 2.39- 1.84 | 6 | 0.904 ( 0.113) | 0.910 ( 0.122) | 0.963 ( 0.450) | 1.75- 1.64 | 6 | 0.881 ( 0.091) | 0.874 ( 0.157) | 0.730 ( 0.301) | 1.58- 1.45 | 6 | 0.918 ( 0.108) | 0.960 ( 0.133) | 0.704 ( 0.124) | 1.45- 1.22 | 6 | 0.943 ( 0.058) | 0.990 ( 0.091) | 0.907 ( 0.216) | 1.22- 1.14 | 6 | 0.912 ( 0.100) | 0.932 ( 0.150) | 0.889 ( 0.548) | 1.09- 1.00 | 6 | 0.889 ( 0.076) | 0.968 ( 0.081) | 0.860 ( 0.497) | 1.00- 0.88 | 6 | 0.935 ( 0.064) | 0.989 ( 0.101) | 0.913 ( 0.296) | 0.88- 0.82 | 6 | 0.939 ( 0.062) | 0.909 ( 0.097) | 1.308 ( 0.394) | 0.82- 0.67 | 10 | 0.942 ( 0.028) | 0.910 ( 0.078) | 1.344 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.67 | 64 | 0.917 ( 0.083) | 0.933 ( 0.119) | 0.964 ( 0.438) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 64 obs out of 64 (total:64,skipped:0) (100.00%) UB - matrix: 0.087753 -0.044924 0.015117 ( 0.000145 0.000095 0.000167 ) 0.062799 0.093439 0.025810 ( 0.000147 0.000097 0.000169 ) 0.047922 0.056903 0.133339 ( 0.000157 0.000103 0.000181 ) M - matrix: 0.013941 0.004653 0.009337 ( 0.000035 0.000021 0.000029 ) 0.004653 0.013987 0.009320 ( 0.000021 0.000023 0.000025 ) 0.009337 0.009320 0.018674 ( 0.000029 0.000025 0.000049 ) unit cell: 7.366(10) 7.341(11) 7.345(12) 119.95(16) 120.12(16) 89.95(12) V = 280.7(7) OTKP changes: 64 1 1 1 OTKP changes: 64 1 1 1 UB - matrix: 0.087913 -0.044820 0.015235 ( 0.000122 0.000080 0.000140 ) 0.062926 0.093376 0.025875 ( 0.000118 0.000077 0.000135 ) 0.048014 0.057104 0.133620 ( 0.000135 0.000088 0.000155 ) M - matrix: 0.013994 0.004677 0.009383 ( 0.000029 0.000017 0.000025 ) 0.004677 0.013989 0.009364 ( 0.000017 0.000019 0.000021 ) 0.009383 0.009364 0.018756 ( 0.000025 0.000021 0.000042 ) UB fit with 64 obs out of 64 (total:64,skipped:0) (100.00%) unit cell: 7.355(9) 7.349(9) 7.338(10) 120.03(13) 120.12(13) 89.96(9) V = 280.0(6) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.896) HKL list info: 454 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 64 obs out of 64 (total:64,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb 0 of 64 peaks identified as outliers and rejected 64 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 64 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 64 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.38 | 6 | 0.891 ( 0.086) | 0.903 ( 0.108) | 0.764 ( 0.166) | 2.38- 2.10 | 6 | 0.909 ( 0.107) | 0.922 ( 0.109) | 0.954 ( 0.440) | 1.83- 1.65 | 6 | 0.862 ( 0.099) | 0.851 ( 0.149) | 0.797 ( 0.417) | 1.64- 1.56 | 6 | 0.955 ( 0.045) | 1.006 ( 0.062) | 0.696 ( 0.151) | 1.45- 1.30 | 6 | 0.918 ( 0.112) | 0.965 ( 0.140) | 0.838 ( 0.238) | 1.22- 1.09 | 6 | 0.933 ( 0.076) | 0.984 ( 0.113) | 1.015 ( 0.386) | 1.09- 1.00 | 6 | 0.916 ( 0.086) | 0.990 ( 0.090) | 0.839 ( 0.344) | 1.00- 0.88 | 6 | 0.935 ( 0.054) | 0.935 ( 0.084) | 0.899 ( 0.296) | 0.88- 0.82 | 6 | 0.951 ( 0.052) | 0.936 ( 0.106) | 1.241 ( 0.482) | 0.82- 0.67 | 10 | 0.943 ( 0.029) | 0.916 ( 0.084) | 1.343 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.67 | 64 | 0.923 ( 0.082) | 0.939 ( 0.115) | 0.964 ( 0.422) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.2 | 28 | 0.977 ( 0.039) | 1.046 ( 0.059) | 1.079 ( 0.431) | 12.4-16.5 | 28 | 1.057 ( 0.379) | 1.082 ( 0.107) | 1.406 ( 1.896) | 16.6-20.6 | 28 | 0.946 ( 0.060) | 1.017 ( 0.089) | 0.992 ( 0.516) | 21.0-24.7 | 28 | 0.956 ( 0.056) | 1.008 ( 0.097) | 0.986 ( 0.432) | 24.7-28.6 | 28 | 0.943 ( 0.081) | 0.997 ( 0.126) | 1.045 ( 0.492) | 29.0-33.6 | 28 | 0.919 ( 0.122) | 0.927 ( 0.132) | 0.857 ( 0.400) | 33.8-36.9 | 28 | 0.941 ( 0.259) | 0.875 ( 0.122) | 1.314 ( 0.965) | 36.9-39.0 | 28 | 0.851 ( 0.084) | 0.832 ( 0.135) | 0.919 ( 0.426) | 39.1-42.0 | 28 | 0.893 ( 0.098) | 0.852 ( 0.148) | 1.052 ( 0.464) | 42.0-49.8 | 24 | 0.881 ( 0.117) | 0.794 ( 0.115) | 1.063 ( 0.528) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 276 | 0.937 ( 0.174) | 0.945 ( 0.149) | 1.071 ( 0.809) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.13 e2 dimension: a=-0.0081 b=1.29 e3 dimension: a=0.0054 b=0.92 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5551 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386802 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693083 lp-corr: 1340780 PROFFITPEAK - Finished at Wed Aug 21 12:28:05 2019 PROFFITMAIN - Started at Wed Aug 21 12:28:05 2019 OTKP changes: 214 2 1 2 OTKP changes: 214 2 1 2 OTKP changes: 214 2 1 2 UB - matrix: 0.087472 -0.046050 0.017299 ( 0.000095 0.000061 0.000092 ) 0.064499 0.092360 0.027205 ( 0.000091 0.000058 0.000088 ) 0.045574 0.057821 0.132137 ( 0.000106 0.000068 0.000102 ) M - matrix: 0.013888 0.004564 0.009290 ( 0.000023 0.000013 0.000018 ) 0.004564 0.013994 0.009356 ( 0.000013 0.000014 0.000014 ) 0.009290 0.009356 0.018500 ( 0.000018 0.000014 0.000028 ) UB fit with 223 obs out of 276 (total:276,skipped:0) (80.80%) unit cell: 7.386(6) 7.371(6) 7.433(7) 120.58(9) 120.42(9) 89.17(7) V = 283.9(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 201 obs out of 212 (total:212,skipped:0) (94.81%) UB - matrix: 0.087473 -0.046072 0.017430 ( 0.000098 0.000061 0.000092 ) 0.064713 0.092370 0.027217 ( 0.000089 0.000055 0.000084 ) 0.045644 0.057902 0.132153 ( 0.000100 0.000062 0.000094 ) M - matrix: 0.013923 0.004590 0.009318 ( 0.000023 0.000013 0.000017 ) 0.004590 0.014008 0.009363 ( 0.000013 0.000014 0.000013 ) 0.009318 0.009363 0.018509 ( 0.000017 0.000013 0.000025 ) unit cell: 7.383(6) 7.367(6) 7.433(6) 120.53(9) 120.44(9) 89.24(7) V = 283.5(4) OTKP changes: 199 1 1 1 OTKP changes: 199 1 1 1 OTKP changes: 199 1 1 1 UB - matrix: 0.087393 -0.045989 0.017481 ( 0.000098 0.000060 0.000092 ) 0.064704 0.092325 0.027257 ( 0.000086 0.000053 0.000081 ) 0.045561 0.057848 0.132074 ( 0.000102 0.000064 0.000096 ) M - matrix: 0.013900 0.004590 0.009309 ( 0.000022 0.000013 0.000017 ) 0.004590 0.013985 0.009353 ( 0.000013 0.000014 0.000013 ) 0.009309 0.009353 0.018492 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.390(6) 7.374(6) 7.437(6) 120.52(9) 120.44(9) 89.27(7) V = 284.2(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.066) HKL list info: 1301 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087392 -0.045989 0.017481 ( 0.000098 0.000060 0.000092 ) 0.064704 0.092325 0.027258 ( 0.000086 0.000053 0.000081 ) 0.045560 0.057848 0.132075 ( 0.000103 0.000064 0.000097 ) M - matrix: 0.013900 0.004590 0.009309 ( 0.000022 0.000013 0.000017 ) 0.004590 0.013985 0.009353 ( 0.000013 0.000014 0.000013 ) 0.009309 0.009353 0.018492 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.390(6) 7.374(6) 7.437(6) 120.52(9) 120.44(9) 89.27(7) V = 284.2(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118090 0.039116 0.078814 ( 0.000075 0.000047 0.000069 ) 0.000036 0.111563 0.056244 ( 0.000075 0.000047 0.000069 ) 0.000027 -0.000046 0.095533 ( 0.000091 0.000057 0.000084 ) M - matrix: 0.013945 0.004623 0.009312 ( 0.000018 0.000010 0.000014 ) 0.004623 0.013976 0.009353 ( 0.000010 0.000011 0.000011 ) 0.009312 0.009353 0.018502 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.372(5) 7.376(5) 7.424(8) 120.45(9) 120.29(9) 89.48(5) V = 283.5(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 64 obs out of 64 (total:64,skipped:0) (100.00%) UB - matrix: 0.087973 -0.044774 0.015321 ( 0.000135 0.000087 0.000153 ) 0.062836 0.093321 0.025752 ( 0.000125 0.000081 0.000142 ) 0.048063 0.057134 0.133667 ( 0.000141 0.000091 0.000161 ) M - matrix: 0.013998 0.004671 0.009390 ( 0.000032 0.000018 0.000026 ) 0.004671 0.013978 0.009354 ( 0.000018 0.000020 0.000021 ) 0.009390 0.009354 0.018765 ( 0.000026 0.000021 0.000044 ) unit cell: 7.356(9) 7.349(9) 7.336(10) 120.00(14) 120.15(14) 89.94(10) V = 279.9(6) OTKP changes: 64 1 1 1 OTKP changes: 64 1 1 1 UB - matrix: 0.088097 -0.044760 0.015407 ( 0.000135 0.000087 0.000154 ) 0.062869 0.093396 0.025761 ( 0.000125 0.000080 0.000142 ) 0.048127 0.057236 0.133815 ( 0.000141 0.000091 0.000160 ) M - matrix: 0.014030 0.004683 0.009417 ( 0.000032 0.000018 0.000026 ) 0.004683 0.014002 0.009375 ( 0.000018 0.000020 0.000021 ) 0.009417 0.009375 0.018808 ( 0.000026 0.000021 0.000044 ) UB fit with 64 obs out of 64 (total:64,skipped:0) (100.00%) unit cell: 7.349(9) 7.344(9) 7.330(10) 120.00(14) 120.17(14) 89.93(10) V = 279.1(6) Run 2 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.838) HKL list info: 440 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.088097 -0.044760 0.015407 ( 0.000135 0.000087 0.000154 ) 0.062869 0.093396 0.025761 ( 0.000125 0.000080 0.000142 ) 0.048127 0.057236 0.133815 ( 0.000141 0.000091 0.000160 ) M - matrix: 0.014030 0.004683 0.009417 ( 0.000032 0.000018 0.000026 ) 0.004683 0.014002 0.009375 ( 0.000018 0.000020 0.000021 ) 0.009417 0.009375 0.018808 ( 0.000026 0.000021 0.000044 ) UB fit with 64 obs out of 64 (total:64,skipped:0) (100.00%) unit cell: 7.349(9) 7.344(9) 7.330(10) 120.00(14) 120.17(14) 89.93(10) V = 279.1(6) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117977 0.039119 0.078777 ( 0.000064 0.000040 0.000062 ) 0.000023 0.111592 0.056181 ( 0.000063 0.000039 0.000061 ) -0.000063 -0.000165 0.095742 ( 0.000084 0.000053 0.000082 ) M - matrix: 0.013919 0.004618 0.009289 ( 0.000015 0.000009 0.000013 ) 0.004618 0.013983 0.009335 ( 0.000009 0.000009 0.000010 ) 0.009289 0.009335 0.018529 ( 0.000013 0.000010 0.000020 ) UB fit with 271 obs out of 276 (total:276,skipped:0) (98.19%) unit cell: 7.371(5) 7.363(4) 7.400(7) 120.31(8) 120.18(8) 89.61(5) V = 282.8(3) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 51 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof 1263 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:28:08 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.066) Run 2 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.838) PROFFIT INFO: signal sum: min=-560.0000 max=8327380.0000 PROFFIT INFO: signal sum lp corr: min=-599.8334 max=1196955.6978 PROFFIT INFO: background sum: min=132.0000 max=7036.0000 PROFFIT INFO: background sum sig2: min=380.0000 max=5272.0000 PROFFIT INFO: num of signal pixels: min=35 max=525 PROFFIT INFO: Inet: min=-959.7334 max=1915129.2500 PROFFIT INFO: sig(Inet): min=64.9740 max=24468.0195 PROFFIT INFO: Inet/sig(Inet): min=-1.59 max=177.60 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 136 468 674 798 860 989 1063 1116 1198 1253 1263 Percent 10.8 37.1 53.4 63.2 68.1 78.3 84.2 88.4 94.9 99.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1263 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 1263 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1915129- 120206 126 405644.34 74.34 100.00 118607- 4242 126 28018.04 19.39 100.00 4204- 2004 126 2835.80 7.07 99.21 2002- 1207 126 1534.08 3.59 45.24 1204- 784 126 977.15 2.16 11.11 781- 505 126 642.14 1.66 9.52 503- 287 126 389.28 1.13 3.97 283- 123 126 194.11 0.53 0.00 119- -8 126 52.98 0.20 0.00 -8- -960 129 -187.83 -0.35 0.00 ------------------------------------------------------------------------------------ 1915129- -960 1263 43905.03 10.94 36.82 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 126 112424.72 17.90 71.43 1.75- 1.28 126 86406.65 20.30 53.97 1.28- 1.08 126 53966.08 13.41 46.03 1.08- 0.94 126 34352.97 11.35 48.41 0.94- 0.85 126 36163.41 10.56 28.57 0.85- 0.77 126 25370.93 8.09 26.19 0.77- 0.71 126 37946.86 10.56 32.54 0.71- 0.65 126 16943.15 5.85 21.43 0.65- 0.60 126 24777.60 7.57 26.19 0.60- 0.47 129 11470.17 4.03 13.95 ------------------------------------------------------------------------------------ 6.55- 0.47 1263 43905.03 10.94 36.82 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:28:08 2019 Sorting 1263 observations 59 unique observations with > 7.00 F2/sig(F2) 1263 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 23 127 Total number of frames 127 Maximum number of 59 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1263 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 7 43 Total number of frames 43 294 observations > 7.00 F2/sig(F2) 294 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 7 43 Total number of frames 43 Removing 'redundancy=1' reflections Average redundancy: 3.5 (Out of 294 removed 38 = 256, unique = 73) 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 256 observations in 2 runs Run # start # end # total # 1 0 33 34 2 0 7 42 Total number of frames 42 73 unique data precomputed (should be 73) 73 unique data with 256 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.5 (Out of 256 removed 0 = 256, unique = 73) 73 unique data precomputed (should be 73) 73 unique data with 256 observations RMS deviation of equivalent data = 0.39721 Rint = 0.40051 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.40051, wR= 0.55396 Trying model 1 (ne=2, no=0)... Results: Rint= 0.29324, wR= 0.38888, Acormin=0.133, Acormax=1.339, Acor_av=0.711 F test: Probability=1.000, F= 1.815 Trying model 2 (ne=2, no=1)... Results: Rint= 0.32313, wR= 0.37889, Acormin=0.135, Acormax=1.288, Acor_av=0.559 F test: Probability=0.000, F= 0.810 Trying model 3 (ne=4, no=0)... Results: Rint= 0.28413, wR= 0.31973, Acormin=0.003, Acormax=1.619, Acor_av=0.602 F test: Probability=0.529, F= 1.011 Trying model 4 (ne=4, no=1)... Results: Rint= 0.30591, wR= 0.33027, Acormin=-0.054, Acormax=1.322, Acor_av=0.508 F test: Probability=0.000, F= 0.857 Trying model 5 (ne=4, no=3)... Results: Rint= 0.69659, wR= 0.59129, Acormin=-0.164, Acormax=0.428, Acor_av=0.054 F test: Probability=0.000, F= 0.158 Trying model 6 (ne=6, no=0)... Results: Rint= 0.30254, wR= 0.33507, Acormin=-0.098, Acormax=1.927, Acor_av=0.387 F test: Probability=0.000, F= 0.823 Trying model 7 (ne=6, no=1)... Results: Rint= 0.36667, wR= 0.37382, Acormin=-0.149, Acormax=1.634, Acor_av=0.322 F test: Probability=0.000, F= 0.550 Trying model 8 (ne=6, no=3)... Results: Rint= 0.51045, wR= 0.49307, Acormin=-0.193, Acormax=0.379, Acor_av=0.065 F test: Probability=0.000, F= 0.271 Trying model 9 (ne=6, no=5)... Results: Rint= 0.16474, wR= 0.18096, Acormin=-0.006, Acormax=0.207, Acor_av=0.074 F test: Probability=1.000, F= 2.403 Final absorption model (ne=2, no=0): Rint= 0.29324, Acormin=0.133, Acormax=1.339, Acor_av=0.711 Combined refinement in use Rint: 0.41304 There are 42 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: 46 pars with 1081 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.39721 Using Levenberg-Marquardt: 0.00010 New wR= 0.19174 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.40051 with corrections 0.15691 Rint for all data: 0.41304 with corrections 0.17358 0 observations identified as outliers and rejected Cycle 2 wR= 0.19174 Using Levenberg-Marquardt: 0.00001 New wR= 0.17513 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.40051 with corrections 0.14168 Rint for all data: 0.41304 with corrections 0.15904 0 observations identified as outliers and rejected Cycle 3 wR= 0.17513 Using Levenberg-Marquardt: 0.00000 New wR= 0.17157 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.40051 with corrections 0.14461 Rint for all data: 0.41304 with corrections 0.16200 0 observations identified as outliers and rejected Cycle 4 wR= 0.17157 Using Levenberg-Marquardt: 0.00000 New wR= 0.17098 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.40051 with corrections 0.14525 Rint for all data: 0.41304 with corrections 0.16258 0 observations identified as outliers and rejected Cycle 5 wR= 0.17098 Using Levenberg-Marquardt: 0.00000 New wR= 0.17019 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.40051 with corrections 0.14558 Rint for all data: 0.41304 with corrections 0.16290 0 observations identified as outliers and rejected Final wR= 0.17019 Final frame scales: Min= 0.5288 Max= 1.9198 Final absorption correction factors: Amin= 0.3690 Amax= 1.3442 PROFFIT INFO: Inet (after scale3 abspack): min=-1533.1700 max=1265687.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=35.4897 max=22920.2832 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/103 1263 reflections read from tmp file 376 reflections are rejected (277 as outliers, 99 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 0 78 61 45 37 15 6 3 3 Initial Chi^2= 2.74571 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.79476 Current error model SIG(F2)^2 = 556.22*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 442.06*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 442.06*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1265688- 117825 126 346130.42 31.19 100.00 114863- 3833 126 25144.51 6.49 83.33 3758- 1813 126 2535.45 2.59 19.84 1804- 1118 126 1419.42 1.84 14.29 1118- 687 126 883.01 1.40 3.97 687- 439 126 565.48 1.11 0.79 439- 263 126 345.43 0.98 0.00 261- 99 126 178.94 0.78 1.59 98- -5 126 47.56 0.36 0.00 -5- -1533 129 -215.34 -0.43 0.00 ------------------------------------------------------------------------------------ 1265688- -1533 1263 37613.42 4.62 22.33 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 126 97695.83 11.83 52.38 1.75- 1.28 126 82830.25 8.13 37.30 1.28- 1.08 126 42945.93 5.70 26.19 1.08- 0.94 126 38091.10 3.98 21.43 0.94- 0.85 126 30027.41 3.67 17.46 0.85- 0.77 126 24314.91 2.92 13.49 0.77- 0.71 126 25931.48 3.62 20.63 0.71- 0.65 126 10121.27 2.23 7.94 0.65- 0.60 126 17426.14 2.65 17.46 0.60- 0.47 129 7467.63 1.55 9.30 ------------------------------------------------------------------------------------ 6.55- 0.47 1263 37613.42 4.62 22.33 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 126 97695.83 11.83 52.38 6.55- 1.28 252 90263.04 9.98 44.84 6.55- 1.08 378 74490.67 8.55 38.62 6.55- 0.94 504 65390.78 7.41 34.33 6.55- 0.85 630 58318.10 6.66 30.95 6.55- 0.77 756 52650.90 6.04 28.04 6.55- 0.71 882 48833.84 5.69 26.98 6.55- 0.65 1008 43994.77 5.26 24.60 6.55- 0.60 1134 41042.70 4.97 23.81 6.55- 0.47 1263 37613.42 4.62 22.33 ------------------------------------------------------------------------------------ 6.55- 0.47 1263 37613.42 4.62 22.33 Scale applied to data: s=0.790083 (maximum obs:1265687.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.163; Rsigma 0.053: data 1263 -> merged 356 With outlier rejection... Rint 0.133; Rsigma 0.053: data 1172 -> merged 356 Rejected total: 91, method kkm 87, method Blessing 4 Completeness direct cell (a, b, c) = (6.564, 6.564, 6.564), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.471255, 6.563816 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.35 - 1.59 22 22 6.18 100.00 136 1.55 - 1.22 22 22 6.05 100.00 133 1.20 - 1.03 22 22 4.91 100.00 108 1.03 - 0.92 22 22 4.68 100.00 103 0.92 - 0.84 22 22 4.27 100.00 94 0.84 - 0.79 22 22 3.82 100.00 84 0.79 - 0.75 22 22 3.50 100.00 77 0.75 - 0.71 22 22 2.82 100.00 62 0.71 - 0.69 22 22 3.00 100.00 66 0.68 - 0.65 25 29 2.92 86.21 73 --------------------------------------------------------------- 7.35 - 0.65 223 227 4.20 98.24 936 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:28:08 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.370511 7.363298 7.399662 120.3129 120.1819 89.6138 1172 Reflections read from file xs2212a.hkl 1172 Reflections used for space-group determination (up to diffraction limit of 0.52A); mean (I/sigma) = 4.34 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 601 594 591 593 893 779 782 1172 N (int>3sigma) = 0 53 52 71 48 88 156 160 227 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.9 26.6 29.9 27.1 Mean int/sigma = 0.0 1.2 1.3 1.7 1.2 1.4 4.2 4.9 4.3 Lattice type: P chosen Volume: 282.79 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 Unitcell: 7.347 7.361 7.363 60.02 60.40 60.15 Niggli form: a.a = 53.973 b.b = 54.190 c.c = 54.218 b.c = 27.084 a.c = 26.718 a.b = 26.919 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.440 CUBIC F-lattice R(int) = 0.250 [ 944] Vol = 1131.2 Cell: 10.383 10.422 10.453 90.30 90.06 90.14 Volume: 1131.17 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 2.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.431 RHOMBOHEDRAL R-lattice R(int) = 0.251 [ 725] Vol = 848.4 Cell: 7.371 7.400 17.995 90.18 89.75 120.18 Volume: 848.38 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.431 RHOMBOHEDRAL R-lattice R(int) = 0.217 [ 218] Vol = 848.4 Trigonal Cell: 7.371 7.400 17.995 90.18 89.75 120.18 Volume: 848.38 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.365 RHOMBOHEDRAL R-lattice R(int) = 0.214 [ 596] Vol = 848.4 Cell: 7.347 7.371 18.087 89.62 90.32 119.97 Volume: 848.38 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.365 RHOMBOHEDRAL R-lattice R(int) = 0.198 [ 165] Vol = 848.4 Trigonal Cell: 7.347 7.371 18.087 89.62 90.32 119.97 Volume: 848.38 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.278 ORTHORHOMBIC I-lattice R(int) = 0.247 [ 710] Vol = 565.6 Cell: 7.347 7.365 10.453 89.83 89.75 89.79 Volume: 565.59 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 1.106 ORTHORHOMBIC I-lattice R(int) = 0.144 [ 602] Vol = 565.6 Cell: 7.363 10.422 7.371 90.11 89.61 90.31 Volume: 565.59 Matrix: 0.0000 1.0000 0.0000 1.0000 1.0000 2.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.387 MONOCLINIC I-lattice R(int) = 0.111 [ 463] Vol = 565.6 Cell: 7.363 7.371 10.422 89.89 90.31 90.39 Volume: 565.59 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.210 MONOCLINIC I-lattice R(int) = 0.258 [ 545] Vol = 565.6 Cell: 7.347 7.365 10.453 90.17 90.25 89.79 Volume: 565.59 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.277 MONOCLINIC I-lattice R(int) = 0.198 [ 442] Vol = 565.6 Cell: 7.365 7.347 10.453 90.25 90.17 89.79 Volume: 565.59 Matrix:-1.0000 0.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.725 MONOCLINIC I-lattice R(int) = 0.198 [ 442] Vol = 565.6 Cell: 10.453 7.347 7.365 89.79 90.17 90.25 Volume: 565.59 Matrix: 1.0000 1.0000 0.0000 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.077 [ 188] Vol = 282.8 Cell: 7.347 7.361 7.363 60.02 60.40 60.15 Volume: 282.79 Matrix: 0.0000 1.0000 1.0000 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 0 591 0 773 779 1172 N (int>3sigma) = 0 0 0 0 71 0 154 156 227 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 28.1 26.6 27.1 Mean int/sigma = 0.0 0.0 0.0 0.0 1.7 0.0 4.3 4.2 4.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.383 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 8 8 98 205 N I>3s 0 0 0 45 0.1 0.1 -0.0 1.6 0.8 0.8 0.1 2.3 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 0.250 871 Fd-3m 1 1 227 C N N N N 37 2284 0.250 933 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.383206 10.421871 10.453431 90.2972 90.0561 90.1418 ZERR 1.00 0.010740 0.020189 0.001868 0.2161 0.0052 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1070447- 114299 129 107 35 3.1 345826.87 32.28 0.117 0.097 107835- 2672 147 133 35 3.8 18495.19 4.78 0.233 0.182 2663- 1667 199 173 35 4.9 1660.26 2.01 0.692 0.695 1615- 1091 147 132 35 3.8 1043.73 1.31 0.547 0.609 1059- 800 140 135 35 3.9 861.81 1.16 0.693 0.767 772- 565 102 99 35 2.8 605.12 0.95 0.681 0.711 564- 413 115 113 35 3.2 468.60 0.91 0.650 0.765 412- 284 98 96 35 2.7 336.13 0.63 0.722 0.975 277- 98 104 102 35 2.9 174.22 0.52 0.799 1.248 96- -939 82 82 41 2.0 -32.76 0.04 0.940 1.946 ------------------------------------------------------------------------------------------- 1070447- -939 1263 1172 356 3.3 34270.38 4.34 0.133 0.112 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-1.29 264 235 38 6.2 83539.83 9.40 0.128 0.098 0.027 1.26-0.98 207 184 36 5.1 47791.10 5.48 0.152 0.134 0.052 0.98-0.84 169 154 35 4.4 17635.75 2.70 0.066 0.047 0.079 0.84-0.76 134 130 36 3.6 21290.64 2.66 0.190 0.194 0.092 0.76-0.71 120 110 37 3.0 21601.61 3.30 0.109 0.099 0.081 0.70-0.66 108 107 35 3.1 11770.56 2.46 0.158 0.136 0.106 0.65-0.62 85 81 35 2.3 10839.06 1.90 0.142 0.152 0.127 0.61-0.58 77 73 35 2.1 11673.22 2.03 0.139 0.151 0.122 0.58-0.55 53 52 35 1.5 13085.60 2.33 0.120 0.119 0.125 0.54-0.47 46 46 34 1.4 4556.35 1.13 0.750 0.895 0.168 ------------------------------------------------------------------------------------------------------ inf-0.47 1263 1172 356 3.3 34270.38 4.34 0.133 0.112 0.053 inf-0.65 1018 936 223 4.2 40120.84 4.93 0.133 0.109 0.048 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-1.29 235 38 38 100.0 6.2 83539.83 21.98 0.128 0.016 1.26-0.98 184 36 36 100.0 5.1 47791.10 10.42 0.152 0.029 0.98-0.84 154 35 35 100.0 4.4 17635.75 4.53 0.066 0.038 0.84-0.76 130 36 36 100.0 3.6 21290.64 4.81 0.190 0.055 0.76-0.71 110 37 37 100.0 3.0 21601.61 5.61 0.109 0.044 0.70-0.66 107 37 35 94.6 3.1 11770.56 3.57 0.158 0.068 0.65-0.62 81 42 35 83.3 2.3 10839.06 2.82 0.142 0.086 0.61-0.58 73 47 35 74.5 2.1 11673.22 2.96 0.139 0.082 0.58-0.55 52 57 35 61.4 1.5 13085.60 3.03 0.120 0.079 0.54-0.47 46 192 34 17.7 1.4 4556.35 1.16 0.750 1.231 -------------------------------------------------------------------------------------------- inf-0.47 1172 558 356 63.8 3.3 34270.38 8.58 0.133 0.033 inf-0.65 936 227 223 98.2 4.2 40120.84 10.07 0.133 0.029 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 2.0 1.0 1.0 0.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 2.0 1.0 1.0 0.0 No constraint UB - matrix: -0.066616 0.008699 0.012322 ( 0.000024 0.000026 0.000029 ) 0.013926 0.013478 0.065194 ( 0.000024 0.000026 0.000029 ) 0.006037 0.066105 -0.014526 ( 0.000037 0.000039 0.000044 ) M - matrix: 0.004668 0.000007 -0.000001 ( 0.000003 0.000003 0.000003 ) 0.000007 0.004627 0.000026 ( 0.000003 0.000005 0.000003 ) -0.000001 0.000026 0.004613 ( 0.000003 0.000003 0.000005 ) Constraint UB - matrix: -0.066616 0.008699 0.012322 ( 0.000024 0.000026 0.000029 ) 0.013926 0.013478 0.065194 ( 0.000024 0.000026 0.000029 ) 0.006037 0.066105 -0.014526 ( 0.000037 0.000039 0.000044 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) unit cell: 10.382(4) 10.427(5) 10.443(5) 90.32(4) 89.99(4) 90.09(4) V = 1130.5(9) unit cell: 10.4173(13) 10.4173(13) 10.4173(13) 90.0 90.0 90.0 V = 1130.5(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.066) Run 2 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.838) PROFFIT INFO: signal sum: min=-560.0000 max=8327380.0000 PROFFIT INFO: signal sum lp corr: min=-599.8334 max=1196955.6978 PROFFIT INFO: background sum: min=132.0000 max=7036.0000 PROFFIT INFO: background sum sig2: min=380.0000 max=5272.0000 PROFFIT INFO: num of signal pixels: min=35 max=525 PROFFIT INFO: Inet: min=-959.7334 max=1915129.2500 PROFFIT INFO: sig(Inet): min=64.9740 max=24468.0195 PROFFIT INFO: Inet/sig(Inet): min=-1.59 max=177.60 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 272 936 1348 1596 1720 1978 2126 2232 2396 2506 2526 Percent 10.8 37.1 53.4 63.2 68.1 78.3 84.2 88.4 94.9 99.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1263 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 1263 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1915129- 120206 126 405644.34 74.34 100.00 118607- 4242 126 28018.04 19.39 100.00 4204- 2004 126 2835.80 7.07 99.21 2002- 1207 126 1534.08 3.59 45.24 1204- 784 126 977.15 2.16 11.11 781- 505 126 642.14 1.66 9.52 503- 287 126 389.28 1.13 3.97 283- 123 126 194.11 0.53 0.00 119- -8 126 52.98 0.20 0.00 -8- -960 129 -187.83 -0.35 0.00 ------------------------------------------------------------------------------------ 1915129- -960 1263 43905.03 10.94 36.82 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 126 108059.26 14.79 68.25 1.64- 1.26 126 89652.93 20.23 54.76 1.26- 1.06 126 68912.74 20.34 73.02 1.04- 0.95 126 36500.07 11.10 22.22 0.95- 0.88 126 37160.48 10.98 46.03 0.88- 0.80 126 32984.32 10.11 31.75 0.80- 0.74 126 15941.62 5.37 23.02 0.74- 0.71 126 25951.64 8.05 18.25 0.71- 0.67 126 22512.37 7.33 24.60 0.67- 0.63 129 2363.93 1.37 6.98 ------------------------------------------------------------------------------------ 6.00- 0.63 1263 43905.03 10.94 36.82 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:28:09 2019 Sorting 1263 observations 39 unique observations with > 7.00 F2/sig(F2) 1263 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 23 127 Total number of frames 127 Maximum number of 39 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1263 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 5 32 Total number of frames 32 294 observations > 7.00 F2/sig(F2) 294 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 5 32 Total number of frames 32 Removing 'redundancy=1' reflections Average redundancy: 6.9 (Out of 294 removed 6 = 288, unique = 42) 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 288 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 5 32 Total number of frames 32 42 unique data precomputed (should be 42) 42 unique data with 288 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.9 (Out of 288 removed 0 = 288, unique = 42) 42 unique data precomputed (should be 42) 42 unique data with 288 observations RMS deviation of equivalent data = 0.27029 Rint = 0.25641 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.25641, wR= 0.34034 Trying model 1 (ne=2, no=0)... Results: Rint= 0.10309, wR= 0.19495, Acormin=0.466, Acormax=1.252, Acor_av=0.908 F test: Probability=1.000, F= 6.061 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12043, wR= 0.17642, Acormin=0.295, Acormax=1.284, Acor_av=0.715 F test: Probability=0.000, F= 0.724 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13444, wR= 0.20024, Acormin=0.255, Acormax=1.399, Acor_av=0.751 F test: Probability=0.000, F= 0.566 Trying model 4 (ne=4, no=1)... Results: Rint= 0.13465, wR= 0.16332, Acormin=0.082, Acormax=1.275, Acor_av=0.606 F test: Probability=0.000, F= 0.557 Trying model 5 (ne=4, no=3)... Results: Rint= 0.12694, wR= 0.17042, Acormin=0.016, Acormax=0.524, Acor_av=0.207 F test: Probability=0.000, F= 0.608 Final absorption model (ne=2, no=0): Rint= 0.10309, Acormin=0.466, Acormax=1.252, Acor_av=0.908 Combined refinement in use Rint: 0.25809 There are 32 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 36 pars with 666 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.27029 Using Levenberg-Marquardt: 0.00010 New wR= 0.14097 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25641 with corrections 0.09704 Rint for all data: 0.25809 with corrections 0.10014 0 observations identified as outliers and rejected Cycle 2 wR= 0.14097 Using Levenberg-Marquardt: 0.00001 New wR= 0.13214 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25641 with corrections 0.09749 Rint for all data: 0.25809 with corrections 0.10057 0 observations identified as outliers and rejected Cycle 3 wR= 0.13214 Using Levenberg-Marquardt: 0.00000 New wR= 0.13189 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25641 with corrections 0.09900 Rint for all data: 0.25809 with corrections 0.10208 0 observations identified as outliers and rejected Cycle 4 wR= 0.13189 Using Levenberg-Marquardt: 0.00000 New wR= 0.13216 Using Levenberg-Marquardt: 0.00000 New wR= 0.13216 Using Levenberg-Marquardt: 0.00001 New wR= 0.13216 Using Levenberg-Marquardt: 0.00010 New wR= 0.13216 Using Levenberg-Marquardt: 0.00100 New wR= 0.13216 Using Levenberg-Marquardt: 0.01000 New wR= 0.13209 Using Levenberg-Marquardt: 0.10000 New wR= 0.13185 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25641 with corrections 0.09955 Rint for all data: 0.25809 with corrections 0.10264 Final wR= 0.13185 Final frame scales: Min= 0.7854 Max= 1.2966 Final absorption correction factors: Amin= 0.6030 Amax= 1.3020 PROFFIT INFO: Inet (after scale3 abspack): min=-938.6388 max=1202017.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=55.9300 max=25772.2910 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/103 1263 reflections read from tmp file 91 reflections are rejected (76 as outliers, 15 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 9 10 15 11 11 11 12 8 52 Initial Chi^2= 0.70011 Cycle 1, Chi^2= 1.03463 Current error model SIG(F2)^2 = 103.24*I_RAW + 4.73*I_BACK+(0.04685*)^2 Cycle 2, Chi^2= 1.04315 Current error model SIG(F2)^2 = 128.70*I_RAW + 1.11*I_BACK+(0.03151*)^2 Cycle 3, Chi^2= 0.99976 Current error model SIG(F2)^2 = 132.57*I_RAW + 1.16*I_BACK+(0.03419*)^2 Cycle 4, Chi^2= 1.00246 Current error model SIG(F2)^2 = 133.61*I_RAW + 1.00*I_BACK+(0.03350*)^2 Cycle 5, Chi^2= 0.99927 Current error model SIG(F2)^2 = 133.64*I_RAW + 1.05*I_BACK+(0.03371*)^2 Cycle 6, Chi^2= 1.00019 Current error model SIG(F2)^2 = 133.62*I_RAW + 1.04*I_BACK+(0.03366*)^2 Cycle 7, Chi^2= 0.99995 Current error model SIG(F2)^2 = 133.62*I_RAW + 1.04*I_BACK+(0.03367*)^2 Final Chi^2= 0.99995 Final error model SIG(F2)^2 = 133.62*I_RAW + 1.04*I_BACK+(0.03367*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1202018- 122107 126 368890.34 24.28 100.00 122027- 3756 126 28430.09 10.53 100.00 3703- 1974 126 2705.99 4.79 88.89 1958- 1136 126 1459.03 3.12 34.92 1132- 758 126 934.10 2.29 11.11 755- 497 126 630.98 1.92 7.94 496- 284 126 380.15 1.75 7.14 282- 114 126 188.76 1.20 0.79 112- -6 126 53.48 0.54 0.00 -7- -939 129 -184.34 -0.73 0.00 ------------------------------------------------------------------------------------ 1202018- -939 1263 40252.58 4.96 35.00 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 126 93285.82 8.04 67.46 1.64- 1.26 126 80239.50 7.37 53.97 1.26- 1.06 126 69921.94 7.58 73.81 1.04- 0.95 126 32303.69 4.12 21.43 0.95- 0.88 126 31903.71 5.22 41.27 0.88- 0.80 126 33229.74 4.65 28.57 0.80- 0.74 126 16085.67 3.11 17.46 0.74- 0.71 126 22379.89 4.36 16.67 0.71- 0.67 126 21746.67 3.98 24.60 0.67- 0.63 129 2332.03 1.22 5.43 ------------------------------------------------------------------------------------ 6.00- 0.63 1263 40252.58 4.96 35.00 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 126 93285.82 8.04 67.46 6.00- 1.26 252 86762.66 7.70 60.71 6.00- 1.06 378 81149.09 7.66 65.08 6.00- 0.95 504 68937.74 6.78 54.17 6.00- 0.88 630 61530.93 6.47 51.59 6.00- 0.80 756 56814.07 6.16 47.75 6.00- 0.74 882 50995.73 5.73 43.42 6.00- 0.71 1008 47418.75 5.56 40.08 6.00- 0.67 1134 44566.29 5.38 38.36 6.00- 0.63 1263 40252.58 4.96 35.00 ------------------------------------------------------------------------------------ 6.00- 0.63 1263 40252.58 4.96 35.00 Scale applied to data: s=0.831934 (maximum obs:1202017.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.103; Rsigma 0.047: data 1263 -> merged 155 With outlier rejection... Rint 0.081; Rsigma 0.048: data 1243 -> merged 155 Rejected total: 20, method kkm 19, method Blessing 1 Completeness direct cell (a, b, c) = (10.417, 10.417, 10.417), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627050, 6.014455 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.35 - 1.76 14 14 7.64 100.00 107 1.74 - 1.27 14 14 9.00 100.00 126 1.26 - 1.06 14 14 10.14 100.00 142 1.05 - 0.97 14 14 8.43 100.00 118 0.95 - 0.88 14 14 9.57 100.00 134 0.87 - 0.81 14 14 8.07 100.00 113 0.80 - 0.76 14 14 8.57 100.00 120 0.76 - 0.72 13 14 7.85 92.86 102 0.72 - 0.69 13 14 8.31 92.86 108 0.69 - 0.65 18 19 7.17 94.74 129 --------------------------------------------------------------- 7.35 - 0.65 142 145 8.44 97.93 1199 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:28:08 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.370511 7.363298 7.399662 120.3129 120.1819 89.6138 1172 Reflections read from file xs2212a.hkl 1172 Reflections used for space-group determination (up to diffraction limit of 0.52A); mean (I/sigma) = 4.34 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 601 594 591 593 893 779 782 1172 N (int>3sigma) = 0 53 52 71 48 88 156 160 227 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.9 26.6 29.9 27.1 Mean int/sigma = 0.0 1.2 1.3 1.7 1.2 1.4 4.2 4.9 4.3 Lattice type: P chosen Volume: 282.79 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 Unitcell: 7.347 7.361 7.363 60.02 60.40 60.15 Niggli form: a.a = 53.973 b.b = 54.190 c.c = 54.218 b.c = 27.084 a.c = 26.718 a.b = 26.919 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.440 CUBIC F-lattice R(int) = 0.250 [ 944] Vol = 1131.2 Cell: 10.383 10.422 10.453 90.30 90.06 90.14 Volume: 1131.17 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 2.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.431 RHOMBOHEDRAL R-lattice R(int) = 0.251 [ 725] Vol = 848.4 Cell: 7.371 7.400 17.995 90.18 89.75 120.18 Volume: 848.38 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.431 RHOMBOHEDRAL R-lattice R(int) = 0.217 [ 218] Vol = 848.4 Trigonal Cell: 7.371 7.400 17.995 90.18 89.75 120.18 Volume: 848.38 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.365 RHOMBOHEDRAL R-lattice R(int) = 0.214 [ 596] Vol = 848.4 Cell: 7.347 7.371 18.087 89.62 90.32 119.97 Volume: 848.38 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.365 RHOMBOHEDRAL R-lattice R(int) = 0.198 [ 165] Vol = 848.4 Trigonal Cell: 7.347 7.371 18.087 89.62 90.32 119.97 Volume: 848.38 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.278 ORTHORHOMBIC I-lattice R(int) = 0.247 [ 710] Vol = 565.6 Cell: 7.347 7.365 10.453 89.83 89.75 89.79 Volume: 565.59 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 1.106 ORTHORHOMBIC I-lattice R(int) = 0.144 [ 602] Vol = 565.6 Cell: 7.363 10.422 7.371 90.11 89.61 90.31 Volume: 565.59 Matrix: 0.0000 1.0000 0.0000 1.0000 1.0000 2.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.387 MONOCLINIC I-lattice R(int) = 0.111 [ 463] Vol = 565.6 Cell: 7.363 7.371 10.422 89.89 90.31 90.39 Volume: 565.59 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 2.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.210 MONOCLINIC I-lattice R(int) = 0.258 [ 545] Vol = 565.6 Cell: 7.347 7.365 10.453 90.17 90.25 89.79 Volume: 565.59 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.277 MONOCLINIC I-lattice R(int) = 0.198 [ 442] Vol = 565.6 Cell: 7.365 7.347 10.453 90.25 90.17 89.79 Volume: 565.59 Matrix:-1.0000 0.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.725 MONOCLINIC I-lattice R(int) = 0.198 [ 442] Vol = 565.6 Cell: 10.453 7.347 7.365 89.79 90.17 90.25 Volume: 565.59 Matrix: 1.0000 1.0000 0.0000 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.077 [ 188] Vol = 282.8 Cell: 7.347 7.361 7.363 60.02 60.40 60.15 Volume: 282.79 Matrix: 0.0000 1.0000 1.0000 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 0 591 0 773 779 1172 N (int>3sigma) = 0 0 0 0 71 0 154 156 227 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 28.1 26.6 27.1 Mean int/sigma = 0.0 0.0 0.0 0.0 1.7 0.0 4.3 4.2 4.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.383 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 8 8 98 205 N I>3s 0 0 0 45 0.1 0.1 -0.0 1.6 0.8 0.8 0.1 2.3 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 0.250 871 Fd-3m 1 1 227 C N N N N 37 2284 0.250 933 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.383206 10.421871 10.453431 90.2972 90.0561 90.1418 ZERR 1.00 0.010740 0.020189 0.001868 0.2161 0.0052 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1116066- 93373 152 137 25 5.5 321886.38 22.88 0.077 0.077 65048- 2257 218 216 25 8.6 5317.58 6.83 0.121 0.128 1970- 861 234 233 25 9.3 1221.70 2.67 0.245 0.308 860- 395 220 220 25 8.8 567.59 1.74 0.425 0.534 389- 90 203 203 25 8.1 265.70 1.28 0.539 0.738 60- -331 236 234 30 7.8 -17.48 0.13 0.927 2.347 ------------------------------------------------------------------------------------------- 1116066- -331 1263 1243 155 8.0 36771.04 4.75 0.081 0.081 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-1.36 222 219 25 8.8 82825.92 7.99 0.086 0.081 0.038 1.30-1.01 229 227 25 9.1 41490.26 4.90 0.087 0.085 0.043 1.00-0.84 226 220 25 8.8 43419.61 5.72 0.055 0.052 0.049 0.84-0.75 223 220 26 8.5 14420.40 3.04 0.088 0.091 0.068 0.74-0.68 199 197 25 7.9 19177.35 3.66 0.081 0.088 0.073 0.68-0.63 164 160 29 5.5 10290.61 2.47 0.135 0.157 0.091 ------------------------------------------------------------------------------------------------------ inf-0.63 1263 1243 155 8.0 36771.04 4.75 0.081 0.081 0.048 inf-0.66 1214 1197 141 8.5 38038.77 4.88 0.081 0.080 0.048 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-1.36 219 25 25 100.0 8.8 82825.92 23.43 0.086 0.021 1.30-1.01 227 25 25 100.0 9.1 41490.26 14.06 0.087 0.020 1.00-0.84 220 25 25 100.0 8.8 43419.61 18.36 0.055 0.024 0.84-0.75 220 26 26 100.0 8.5 14420.40 8.29 0.088 0.027 0.74-0.68 197 27 25 92.6 7.9 19177.35 10.56 0.081 0.028 0.68-0.63 160 34 29 85.3 5.5 10290.61 6.62 0.135 0.043 -------------------------------------------------------------------------------------------- inf-0.63 1243 162 155 95.7 8.0 36771.04 13.94 0.081 0.022 inf-0.66 1197 143 141 98.6 8.5 38038.77 14.38 0.081 0.022 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:34:47 2019) ID: 3668; threads 40; handles 811; mem 515216.00 (1204688.00)kB; time: 1w 4d 22h 45m 34s MEMORY INFO: Memory PF:64.0, Ph:511.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.1,peak PF: 700.2, WS: 471.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:66.0, Ph:513.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.9,peak PF: 700.2, WS: 472.8, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:34:47 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000100 0.000065 0.000097 ) 0.064809 0.092374 0.027273 ( 0.000092 0.000059 0.000089 ) 0.045523 0.057900 0.132205 ( 0.000106 0.000068 0.000102 ) 7.38096 ( 0.00678 ) 7.36649 ( 0.00664 ) 7.42630 ( 0.00687 ) 120.52449 ( 0.09662 ) 120.40327 ( 0.09711 ) 89.27095 ( 0.07380 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:34:47 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000100 0.000065 0.000097 ) 0.064809 0.092374 0.027273 ( 0.000092 0.000059 0.000089 ) 0.045523 0.057900 0.132205 ( 0.000106 0.000068 0.000102 ) M - matrix: 0.013893 0.004573 0.009271 ( 0.000023 0.000014 0.000018 ) 0.004573 0.013991 0.009345 ( 0.000014 0.000015 0.000014 ) 0.009271 0.009345 0.018476 ( 0.000018 0.000014 0.000028 ) unit cell: 7.381(7) 7.366(7) 7.426(7) 120.52(10) 120.40(10) 89.27(7) V = 283.3(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb PROFFITPEAK info: 294 peaks in the peak location table UB fit with 30 obs out of 146 (total:146,skipped:0) (20.55%) UB - matrix: 0.086209 -0.046870 0.015220 ( 0.001060 0.000543 0.001188 ) 0.062713 0.091929 0.026044 ( 0.000873 0.000447 0.000979 ) 0.046553 0.058149 0.133692 ( 0.001521 0.000780 0.001706 ) M - matrix: 0.013532 0.004431 0.009169 ( 0.000256 0.000145 0.000250 ) 0.004431 0.014029 0.009455 ( 0.000145 0.000133 0.000179 ) 0.009169 0.009455 0.018784 ( 0.000250 0.000179 0.000460 ) unit cell: 7.45(7) 7.37(7) 7.37(10) 121(1) 120(1) 88.8(7) V = 284(6) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 146 #indexed refl 134, indexation with best UB: 91.7808% Lattice: 7.3895 7.3683 7.3406 120.157 119.999 89.721 282.637 Rotation: -23.868 24.070 -35.433 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 136 obs out of 146 (total:146,skipped:0) (93.15%) UB - matrix: 0.087392 -0.045107 0.014482 ( 0.000151 0.000126 0.000180 ) 0.062092 0.092800 0.025219 ( 0.000184 0.000154 0.000219 ) 0.047884 0.056952 0.133451 ( 0.000166 0.000139 0.000198 ) M - matrix: 0.013786 0.004547 0.009222 ( 0.000038 0.000026 0.000032 ) 0.004547 0.013890 0.009287 ( 0.000026 0.000035 0.000031 ) 0.009222 0.009287 0.018655 ( 0.000032 0.000031 0.000054 ) unit cell: 7.384(12) 7.369(14) 7.340(14) 120.1(2) 119.98(18) 89.73(14) V = 282.6(9) OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 UB fit with 136 obs out of 146 (total:146,skipped:0) (93.15%) UB - matrix: 0.087392 -0.045108 0.014477 ( 0.000152 0.000126 0.000180 ) 0.062089 0.092797 0.025212 ( 0.000184 0.000153 0.000219 ) 0.047883 0.056951 0.133448 ( 0.000166 0.000138 0.000198 ) M - matrix: 0.013785 0.004547 0.009221 ( 0.000038 0.000026 0.000032 ) 0.004547 0.013889 0.009286 ( 0.000026 0.000034 0.000031 ) 0.009221 0.009286 0.018654 ( 0.000032 0.000031 0.000054 ) unit cell: 7.384(12) 7.369(14) 7.340(14) 120.1(2) 119.98(18) 89.73(14) V = 282.6(9) OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 146 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Run 2 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 726 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087392 -0.045108 0.014477 ( 0.000152 0.000126 0.000180 ) 0.062089 0.092797 0.025212 ( 0.000184 0.000153 0.000219 ) 0.047883 0.056950 0.133447 ( 0.000166 0.000138 0.000198 ) M - matrix: 0.013785 0.004547 0.009220 ( 0.000038 0.000026 0.000032 ) 0.004547 0.013889 0.009286 ( 0.000026 0.000034 0.000031 ) 0.009220 0.009286 0.018653 ( 0.000032 0.000031 0.000054 ) UB fit with 136 obs out of 146 (total:146,skipped:0) (93.15%) unit cell: 7.384(12) 7.369(14) 7.340(14) 120.1(2) 119.98(18) 89.73(14) V = 282.6(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 135 obs out of 146 (total:146,skipped:0) (92.47%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb 0 of 130 peaks identified as outliers and rejected 130 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 130 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 130 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.90- 2.37 | 13 | 0.845 ( 0.089) | 0.836 ( 0.121) | 0.955 ( 0.451) | 2.37- 1.76 | 13 | 0.862 ( 0.116) | 0.843 ( 0.172) | 0.944 ( 0.443) | 1.75- 1.64 | 13 | 0.902 ( 0.069) | 0.900 ( 0.133) | 0.847 ( 0.423) | 1.58- 1.45 | 13 | 0.937 ( 0.098) | 0.978 ( 0.127) | 0.883 ( 0.331) | 1.35- 1.22 | 13 | 0.926 ( 0.044) | 0.952 ( 0.074) | 1.023 ( 0.492) | 1.20- 1.09 | 13 | 0.937 ( 0.067) | 0.961 ( 0.111) | 0.919 ( 0.396) | 1.09- 1.00 | 13 | 0.929 ( 0.079) | 0.976 ( 0.091) | 0.919 ( 0.338) | 1.00- 0.86 | 13 | 0.938 ( 0.070) | 0.924 ( 0.092) | 1.124 ( 0.423) | 0.86- 0.73 | 13 | 0.939 ( 0.031) | 0.914 ( 0.097) | 1.350 ( 0.476) | 0.73- 0.65 | 13 | 0.924 ( 0.040) | 0.865 ( 0.082) | 1.509 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.90- 0.65 | 130 | 0.914 ( 0.081) | 0.915 ( 0.124) | 1.047 ( 0.478) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) UB - matrix: 0.087489 -0.045081 0.014595 ( 0.000077 0.000068 0.000096 ) 0.062345 0.093203 0.025483 ( 0.000077 0.000068 0.000096 ) 0.048243 0.057046 0.133682 ( 0.000074 0.000065 0.000092 ) M - matrix: 0.013869 0.004619 0.009315 ( 0.000018 0.000012 0.000015 ) 0.004619 0.013973 0.009343 ( 0.000012 0.000016 0.000014 ) 0.009315 0.009343 0.018733 ( 0.000015 0.000014 0.000025 ) unit cell: 7.380(6) 7.350(6) 7.337(6) 120.07(9) 120.11(9) 89.83(7) V = 281.1(4) OTKP changes: 130 1 1 1 OTKP changes: 130 1 1 1 UB - matrix: 0.087446 -0.045075 0.014543 ( 0.000075 0.000066 0.000094 ) 0.062360 0.093077 0.025491 ( 0.000075 0.000066 0.000094 ) 0.048146 0.057066 0.133643 ( 0.000063 0.000055 0.000078 ) M - matrix: 0.013854 0.004610 0.009296 ( 0.000017 0.000011 0.000014 ) 0.004610 0.013952 0.009344 ( 0.000011 0.000015 0.000013 ) 0.009296 0.009344 0.018722 ( 0.000014 0.000013 0.000022 ) UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) unit cell: 7.380(6) 7.360(6) 7.340(5) 120.13(8) 120.05(8) 89.82(7) V = 281.5(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.979) HKL list info: 724 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087446 -0.045075 0.014543 ( 0.000075 0.000066 0.000094 ) 0.062360 0.093077 0.025491 ( 0.000075 0.000066 0.000094 ) 0.048146 0.057066 0.133643 ( 0.000063 0.000055 0.000078 ) M - matrix: 0.013854 0.004610 0.009296 ( 0.000017 0.000011 0.000014 ) 0.004610 0.013952 0.009344 ( 0.000011 0.000015 0.000013 ) 0.009296 0.009344 0.018722 ( 0.000014 0.000013 0.000022 ) UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) unit cell: 7.380(6) 7.360(6) 7.340(5) 120.13(8) 120.05(8) 89.82(7) V = 281.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb 0 of 130 peaks identified as outliers and rejected 130 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 130 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 130 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.38 | 13 | 0.860 ( 0.100) | 0.856 ( 0.135) | 0.999 ( 0.439) | 2.38- 1.75 | 13 | 0.874 ( 0.106) | 0.870 ( 0.152) | 0.956 ( 0.503) | 1.75- 1.58 | 13 | 0.897 ( 0.088) | 0.893 ( 0.160) | 0.916 ( 0.405) | 1.58- 1.35 | 13 | 0.940 ( 0.099) | 0.977 ( 0.126) | 0.971 ( 0.497) | 1.35- 1.16 | 13 | 0.920 ( 0.056) | 0.946 ( 0.099) | 0.963 ( 0.436) | 1.16- 1.09 | 13 | 0.911 ( 0.063) | 0.990 ( 0.101) | 0.798 ( 0.294) | 1.06- 0.91 | 13 | 0.969 ( 0.055) | 0.999 ( 0.081) | 1.005 ( 0.326) | 0.89- 0.87 | 13 | 0.947 ( 0.051) | 0.928 ( 0.106) | 1.203 ( 0.423) | 0.86- 0.73 | 13 | 0.940 ( 0.031) | 0.901 ( 0.085) | 1.353 ( 0.413) | 0.73- 0.65 | 13 | 0.924 ( 0.041) | 0.874 ( 0.091) | 1.477 ( 0.518) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.65 | 130 | 0.918 ( 0.080) | 0.923 ( 0.127) | 1.064 ( 0.476) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-11.4 | 34 | 0.975 ( 0.038) | 1.024 ( 0.084) | 1.108 ( 0.455) | 11.6-15.9 | 34 | 1.037 ( 0.346) | 1.069 ( 0.098) | 1.417 ( 1.740) | 16.2-20.5 | 34 | 0.949 ( 0.062) | 1.010 ( 0.097) | 1.016 ( 0.472) | 20.6-24.2 | 34 | 0.953 ( 0.053) | 1.007 ( 0.083) | 0.910 ( 0.391) | 24.2-27.5 | 34 | 0.946 ( 0.073) | 0.990 ( 0.114) | 1.063 ( 0.476) | 27.6-32.4 | 34 | 0.930 ( 0.105) | 0.947 ( 0.131) | 0.983 ( 0.504) | 32.4-36.4 | 34 | 0.930 ( 0.240) | 0.885 ( 0.128) | 1.201 ( 0.847) | 36.4-38.6 | 34 | 0.853 ( 0.089) | 0.823 ( 0.124) | 0.993 ( 0.512) | 38.6-41.3 | 34 | 0.891 ( 0.088) | 0.852 ( 0.141) | 1.102 ( 0.497) | 41.6-49.8 | 36 | 0.868 ( 0.115) | 0.782 ( 0.123) | 1.095 ( 0.556) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 342 | 0.933 ( 0.160) | 0.938 ( 0.147) | 1.089 ( 0.761) | Fitted profile normalization line parameters e1 dimension: a=-0.0036 b=1.14 e2 dimension: a=-0.0085 b=1.29 e3 dimension: a=0.0075 b=0.85 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5551 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386273 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1337465 PROFFITPEAK - Finished at Wed Aug 21 12:34:53 2019 PROFFITMAIN - Started at Wed Aug 21 12:34:53 2019 OTKP changes: 226 2 1 2 OTKP changes: 226 2 1 2 OTKP changes: 226 2 1 2 UB - matrix: 0.087463 -0.046066 0.017226 ( 0.000096 0.000061 0.000093 ) 0.064434 0.092352 0.027228 ( 0.000091 0.000058 0.000088 ) 0.045592 0.057698 0.132038 ( 0.000109 0.000069 0.000105 ) M - matrix: 0.013880 0.004552 0.009281 ( 0.000023 0.000013 0.000018 ) 0.004552 0.013980 0.009339 ( 0.000013 0.000014 0.000014 ) 0.009281 0.009339 0.018472 ( 0.000018 0.000014 0.000028 ) UB fit with 233 obs out of 342 (total:342,skipped:0) (68.13%) unit cell: 7.389(7) 7.373(6) 7.439(7) 120.58(10) 120.44(10) 89.13(7) V = 284.3(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 202 obs out of 212 (total:212,skipped:0) (95.28%) UB - matrix: 0.087485 -0.046108 0.017420 ( 0.000099 0.000061 0.000091 ) 0.064739 0.092347 0.027250 ( 0.000087 0.000054 0.000081 ) 0.045711 0.057839 0.132156 ( 0.000104 0.000065 0.000097 ) M - matrix: 0.013934 0.004589 0.009329 ( 0.000023 0.000013 0.000018 ) 0.004589 0.013999 0.009357 ( 0.000013 0.000014 0.000013 ) 0.009329 0.009357 0.018511 ( 0.000018 0.000013 0.000026 ) unit cell: 7.383(6) 7.368(6) 7.435(6) 120.52(9) 120.49(9) 89.21(7) V = 283.5(4) OTKP changes: 200 1 1 1 OTKP changes: 200 1 1 1 OTKP changes: 200 1 1 1 UB - matrix: 0.087352 -0.045947 0.017473 ( 0.000098 0.000061 0.000092 ) 0.064657 0.092292 0.027270 ( 0.000086 0.000053 0.000081 ) 0.045522 0.057794 0.131992 ( 0.000102 0.000063 0.000096 ) M - matrix: 0.013883 0.004585 0.009298 ( 0.000022 0.000013 0.000017 ) 0.004585 0.013969 0.009342 ( 0.000013 0.000013 0.000013 ) 0.009298 0.009342 0.018471 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.395(6) 7.378(6) 7.441(6) 120.52(9) 120.44(9) 89.27(7) V = 284.7(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.114) HKL list info: 1304 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087351 -0.045946 0.017473 ( 0.000098 0.000061 0.000092 ) 0.064657 0.092292 0.027270 ( 0.000086 0.000053 0.000081 ) 0.045521 0.057794 0.131992 ( 0.000102 0.000063 0.000096 ) M - matrix: 0.013883 0.004585 0.009298 ( 0.000022 0.000013 0.000017 ) 0.004585 0.013969 0.009342 ( 0.000013 0.000013 0.000013 ) 0.009298 0.009342 0.018471 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.395(6) 7.378(6) 7.441(6) 120.52(9) 120.44(9) 89.27(7) V = 284.7(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118019 0.039091 0.078769 ( 0.000075 0.000047 0.000069 ) 0.000036 0.111497 0.056215 ( 0.000075 0.000047 0.000070 ) 0.000027 -0.000046 0.095472 ( 0.000090 0.000056 0.000084 ) M - matrix: 0.013929 0.004618 0.009301 ( 0.000018 0.000010 0.000014 ) 0.004618 0.013960 0.009343 ( 0.000010 0.000011 0.000011 ) 0.009301 0.009343 0.018480 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.376(5) 7.381(5) 7.429(8) 120.46(9) 120.29(9) 89.48(5) V = 284.1(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) UB - matrix: 0.087485 -0.045025 0.014608 ( 0.000078 0.000067 0.000094 ) 0.062378 0.093114 0.025508 ( 0.000072 0.000062 0.000087 ) 0.048202 0.057108 0.133696 ( 0.000064 0.000055 0.000077 ) M - matrix: 0.013868 0.004622 0.009313 ( 0.000017 0.000011 0.000014 ) 0.004622 0.013959 0.009352 ( 0.000011 0.000014 0.000013 ) 0.009313 0.009352 0.018739 ( 0.000014 0.000013 0.000021 ) unit cell: 7.379(6) 7.359(6) 7.339(5) 120.12(8) 120.08(8) 89.84(6) V = 281.4(4) OTKP changes: 130 1 1 1 OTKP changes: 130 1 1 1 UB - matrix: 0.087517 -0.045026 0.014630 ( 0.000078 0.000068 0.000094 ) 0.062385 0.093138 0.025511 ( 0.000072 0.000062 0.000087 ) 0.048217 0.057136 0.133734 ( 0.000063 0.000055 0.000076 ) M - matrix: 0.013876 0.004625 0.009320 ( 0.000017 0.000011 0.000014 ) 0.004625 0.013967 0.009358 ( 0.000011 0.000014 0.000013 ) 0.009320 0.009358 0.018750 ( 0.000014 0.000013 0.000021 ) UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) unit cell: 7.378(6) 7.357(6) 7.338(5) 120.12(8) 120.08(8) 89.83(6) V = 281.2(4) Run 2 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.964) HKL list info: 714 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087517 -0.045026 0.014630 ( 0.000078 0.000068 0.000094 ) 0.062385 0.093138 0.025511 ( 0.000072 0.000062 0.000087 ) 0.048217 0.057136 0.133734 ( 0.000063 0.000055 0.000076 ) M - matrix: 0.013876 0.004625 0.009320 ( 0.000017 0.000011 0.000014 ) 0.004625 0.013967 0.009358 ( 0.000011 0.000014 0.000013 ) 0.009320 0.009358 0.018750 ( 0.000014 0.000013 0.000021 ) UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) unit cell: 7.378(6) 7.357(6) 7.338(5) 120.12(8) 120.08(8) 89.83(6) V = 281.2(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117848 0.039305 0.079136 ( 0.000076 0.000066 0.000092 ) 0.000012 0.111473 0.056071 ( 0.000070 0.000061 0.000085 ) 0.000025 0.000026 0.096675 ( 0.000060 0.000052 0.000073 ) M - matrix: 0.013888 0.004633 0.009329 ( 0.000018 0.000011 0.000014 ) 0.004633 0.013971 0.009363 ( 0.000011 0.000015 0.000013 ) 0.009329 0.009363 0.018752 ( 0.000014 0.000013 0.000022 ) UB fit with 130 obs out of 130 (total:130,skipped:0) (100.00%) unit cell: 7.376(5) 7.357(5) 7.339(6) 120.12(8) 120.09(9) 89.85(6) V = 281.1(3) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117818 0.039084 0.078770 ( 0.000054 0.000037 0.000054 ) 0.000018 0.111510 0.056168 ( 0.000051 0.000035 0.000051 ) -0.000071 -0.000203 0.095841 ( 0.000072 0.000049 0.000072 ) M - matrix: 0.013881 0.004607 0.009275 ( 0.000013 0.000008 0.000011 ) 0.004607 0.013962 0.009323 ( 0.000008 0.000008 0.000008 ) 0.009275 0.009323 0.018545 ( 0.000011 0.000008 0.000017 ) UB fit with 337 obs out of 342 (total:342,skipped:0) (98.54%) unit cell: 7.378(4) 7.365(4) 7.390(6) 120.26(7) 120.15(7) 89.66(4) V = 283.0(3) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 52 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof 1527 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:34:56 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.114) Run 2 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.964) PROFFIT INFO: signal sum: min=-552.0000 max=8391635.0000 PROFFIT INFO: signal sum lp corr: min=-593.0519 max=1179168.2505 PROFFIT INFO: background sum: min=123.0000 max=8027.0000 PROFFIT INFO: background sum sig2: min=360.0000 max=5174.0000 PROFFIT INFO: num of signal pixels: min=36 max=515 PROFFIT INFO: Inet: min=-948.8831 max=1886669.2500 PROFFIT INFO: sig(Inet): min=64.7320 max=24238.9629 PROFFIT INFO: Inet/sig(Inet): min=-1.59 max=176.60 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 156 541 800 955 1030 1193 1291 1350 1446 1514 1527 Percent 10.2 35.4 52.4 62.5 67.5 78.1 84.5 88.4 94.7 99.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1527 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 1527 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1886669- 126276 152 403356.66 76.31 100.00 125322- 4246 152 27684.28 19.13 100.00 4236- 2100 152 2904.22 7.21 100.00 2098- 1235 152 1604.41 3.79 50.66 1232- 806 152 1012.74 2.14 10.53 802- 554 152 676.17 1.68 7.24 553- 317 152 428.52 1.29 7.24 316- 128 152 215.94 0.60 0.66 128- 1 152 62.30 0.22 0.00 1- -949 159 -157.22 -0.30 0.00 ------------------------------------------------------------------------------------ 1886669- -949 1527 43577.39 11.16 37.46 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 152 93723.86 15.97 69.08 1.64- 1.26 152 84513.28 19.79 57.24 1.26- 1.06 152 56260.23 14.51 51.32 1.06- 0.92 152 28503.23 9.73 42.11 0.92- 0.83 152 48088.01 13.28 30.92 0.83- 0.76 152 30753.30 9.64 30.92 0.76- 0.69 152 41814.61 11.68 33.55 0.69- 0.64 152 21946.30 6.70 22.37 0.64- 0.58 152 13530.98 4.81 21.71 0.58- 0.46 159 17826.04 5.68 16.35 ------------------------------------------------------------------------------------ 6.55- 0.46 1527 43577.39 11.16 37.46 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:34:56 2019 Sorting 1527 observations 69 unique observations with > 7.00 F2/sig(F2) 1527 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 49 153 Total number of frames 153 Maximum number of 69 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1527 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 16 52 Total number of frames 52 365 observations > 7.00 F2/sig(F2) 365 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 16 52 Total number of frames 52 Removing 'redundancy=1' reflections Average redundancy: 3.8 (Out of 365 removed 42 = 323, unique = 85) 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 323 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 16 52 Total number of frames 52 85 unique data precomputed (should be 85) 85 unique data with 323 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.8 (Out of 323 removed 0 = 323, unique = 85) 85 unique data precomputed (should be 85) 85 unique data with 323 observations RMS deviation of equivalent data = 0.40074 Rint = 0.39333 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.39333, wR= 0.52462 Trying model 1 (ne=2, no=0)... Results: Rint= 0.27739, wR= 0.37508, Acormin=0.130, Acormax=1.348, Acor_av=0.664 F test: Probability=1.000, F= 1.968 Trying model 2 (ne=2, no=1)... Results: Rint= 0.32764, wR= 0.39170, Acormin=0.159, Acormax=1.247, Acor_av=0.503 F test: Probability=0.000, F= 0.708 Trying model 3 (ne=4, no=0)... Results: Rint= 0.28403, wR= 0.34346, Acormin=0.082, Acormax=1.731, Acor_av=0.519 F test: Probability=0.000, F= 0.917 Trying model 4 (ne=4, no=1)... Results: Rint= 0.31456, wR= 0.36046, Acormin=0.063, Acormax=1.227, Acor_av=0.457 F test: Probability=0.000, F= 0.738 Trying model 5 (ne=4, no=3)... Results: Rint= 0.72162, wR= 0.63546, Acormin=-0.119, Acormax=0.405, Acor_av=0.064 F test: Probability=0.000, F= 0.136 Trying model 6 (ne=6, no=0)... Results: Rint= 0.30381, wR= 0.35432, Acormin=-0.134, Acormax=2.063, Acor_av=0.341 F test: Probability=0.000, F= 0.755 Trying model 7 (ne=6, no=1)... Results: Rint= 0.34240, wR= 0.38428, Acormin=-0.082, Acormax=1.755, Acor_av=0.306 F test: Probability=0.000, F= 0.586 Trying model 8 (ne=6, no=3)... Results: Rint= 0.62996, wR= 0.59012, Acormin=-0.134, Acormax=0.416, Acor_av=0.058 F test: Probability=0.000, F= 0.167 Trying model 9 (ne=6, no=5)... Results: Rint= 0.19344, wR= 0.21434, Acormin=-0.021, Acormax=0.156, Acor_av=0.055 F test: Probability=1.000, F= 1.677 Trying model 10 (ne=8, no=0)... Results: Rint= 0.37836, wR= 0.39758, Acormin=-0.163, Acormax=1.505, Acor_av=0.182 F test: Probability=0.000, F= 0.448 Trying model 11 (ne=8, no=1)... Results: Rint= 0.43568, wR= 0.43638, Acormin=-0.191, Acormax=1.183, Acor_av=0.144 F test: Probability=0.000, F= 0.332 Trying model 12 (ne=8, no=3)... Results: Rint= 0.20038, wR= 0.22041, Acormin=-0.016, Acormax=0.181, Acor_av=0.056 F test: Probability=0.998, F= 1.513 Trying model 13 (ne=8, no=5)... Results: Rint= 0.15386, wR= 0.17217, Acormin=-0.004, Acormax=0.181, Acor_av=0.064 F test: Probability=1.000, F= 2.413 Trying model 14 (ne=8, no=7)... Results: Rint= 0.11368, wR= 0.14811, Acormin=0.009, Acormax=0.354, Acor_av=0.086 F test: Probability=1.000, F= 4.038 Final absorption model (ne=2, no=0): Rint= 0.27739, Acormin=0.130, Acormax=1.348, Acor_av=0.664 Combined refinement in use Rint: 0.40694 There are 52 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 56 pars with 1596 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.40074 Using Levenberg-Marquardt: 0.00010 New wR= 0.20068 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.39333 with corrections 0.16877 Rint for all data: 0.40694 with corrections 0.18461 0 observations identified as outliers and rejected Cycle 2 wR= 0.20068 Using Levenberg-Marquardt: 0.00001 New wR= 0.18283 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.39333 with corrections 0.15035 Rint for all data: 0.40694 with corrections 0.16686 0 observations identified as outliers and rejected Cycle 3 wR= 0.18283 Using Levenberg-Marquardt: 0.00000 New wR= 0.17592 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.39333 with corrections 0.14734 Rint for all data: 0.40694 with corrections 0.16397 0 observations identified as outliers and rejected Cycle 4 wR= 0.17592 Using Levenberg-Marquardt: 0.00000 New wR= 0.17270 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.39333 with corrections 0.14418 Rint for all data: 0.40694 with corrections 0.16081 0 observations identified as outliers and rejected Cycle 5 wR= 0.17270 Using Levenberg-Marquardt: 0.00000 New wR= 0.16927 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.39333 with corrections 0.14131 Rint for all data: 0.40694 with corrections 0.15799 0 observations identified as outliers and rejected Final wR= 0.16927 Final frame scales: Min= 0.3998 Max= 1.2806 Final absorption correction factors: Amin= 0.3843 Amax= 1.2960 PROFFIT INFO: Inet (after scale3 abspack): min=-1517.5925 max=1421989.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=40.4561 max=24020.5313 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/103 1527 reflections read from tmp file 438 reflections are rejected (345 as outliers, 93 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 80 66 46 38 31 10 5 1 5 Initial Chi^2= 2.61273 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.71968 Current error model SIG(F2)^2 = 583.72*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 420.09*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 420.09*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1421990- 117881 152 354996.60 31.54 100.00 113094- 3822 152 25076.24 6.78 84.87 3765- 1867 152 2576.01 2.64 25.66 1861- 1104 152 1466.23 1.96 16.45 1100- 722 152 900.66 1.43 2.63 722- 473 152 597.57 1.13 1.32 473- 281 152 369.15 1.05 0.66 280- 116 152 201.67 0.87 1.97 115- 2 152 56.03 0.45 1.32 1- -1518 159 -186.67 -0.38 0.00 ------------------------------------------------------------------------------------ 1421990- -1518 1527 38427.52 4.72 23.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 152 89843.32 10.54 50.66 1.64- 1.26 152 82749.04 8.39 41.45 1.26- 1.06 152 46178.69 6.00 31.58 1.06- 0.92 152 33707.22 3.58 18.42 0.92- 0.83 152 38546.15 4.63 19.08 0.83- 0.76 152 26807.84 3.50 17.76 0.76- 0.69 152 30338.27 4.10 18.42 0.69- 0.64 152 16132.72 2.58 13.82 0.64- 0.58 152 10276.13 1.87 9.87 0.58- 0.46 159 10960.76 2.17 13.21 ------------------------------------------------------------------------------------ 6.55- 0.46 1527 38427.52 4.72 23.38 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 152 89843.32 10.54 50.66 6.55- 1.26 304 86296.18 9.46 46.05 6.55- 1.06 456 72923.68 8.31 41.23 6.55- 0.92 608 63119.57 7.12 35.53 6.55- 0.83 760 58204.88 6.63 32.24 6.55- 0.76 912 52972.04 6.10 29.82 6.55- 0.69 1064 49738.65 5.82 28.20 6.55- 0.64 1216 45537.90 5.41 26.40 6.55- 0.58 1368 41619.93 5.02 24.56 6.55- 0.46 1527 38427.52 4.72 23.38 ------------------------------------------------------------------------------------ 6.55- 0.46 1527 38427.52 4.72 23.38 Scale applied to data: s=0.703239 (maximum obs:1421989.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.158; Rsigma 0.051: data 1527 -> merged 383 With outlier rejection... Rint 0.126; Rsigma 0.052: data 1438 -> merged 383 Rejected total: 89, method kkm 84, method Blessing 5 Completeness direct cell (a, b, c) = (6.566, 6.566, 6.566), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.457444, 6.565559 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.38 - 1.59 22 22 7.14 100.00 157 1.55 - 1.22 22 22 6.95 100.00 153 1.20 - 1.03 22 22 6.14 100.00 135 1.03 - 0.92 22 22 5.45 100.00 120 0.92 - 0.84 22 22 5.00 100.00 110 0.84 - 0.79 22 22 4.50 100.00 99 0.79 - 0.75 22 22 4.41 100.00 97 0.75 - 0.71 22 22 3.32 100.00 73 0.71 - 0.69 22 22 3.55 100.00 78 0.68 - 0.65 28 31 3.43 90.32 96 --------------------------------------------------------------- 7.38 - 0.65 226 229 4.95 98.69 1118 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:34:56 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.378044 7.364880 7.390205 120.2630 120.1524 89.6561 1438 Reflections read from file xs2212a.hkl 1438 Reflections used for space-group determination (up to diffraction limit of 0.59A); mean (I/sigma) = 4.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 738 733 721 728 1096 956 958 1438 N (int>3sigma) = 0 85 78 105 71 134 200 208 302 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.9 22.2 25.8 24.4 Mean int/sigma = 0.0 1.4 1.4 1.8 1.3 1.5 4.0 4.8 4.4 Lattice type: P chosen Volume: 283.02 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.348 7.365 7.367 119.97 90.13 119.70 Niggli form: a.a = 53.996 b.b = 54.241 c.c = 54.274 b.c = -27.104 a.c = -0.123 a.b = -26.811 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.498 CUBIC F-lattice R(int) = 0.225 [ 1204] Vol = 1132.1 Cell: 10.393 10.456 10.417 89.84 89.85 90.10 Volume: 1132.07 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.497 RHOMBOHEDRAL R-lattice R(int) = 0.209 [ 879] Vol = 849.1 Cell: 7.365 7.348 18.061 90.00 90.15 119.70 Volume: 849.06 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.497 RHOMBOHEDRAL R-lattice R(int) = 0.235 [ 269] Vol = 849.1 Trigonal Cell: 7.365 7.348 18.061 90.00 90.15 119.70 Volume: 849.06 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.538 TETRAGONAL I-lattice R(int) = 0.165 [ 869] Vol = 566.0 Cell: 7.390 7.369 10.393 89.82 89.97 90.21 Volume: 566.04 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.552 TETRAGONAL I-lattice R(int) = 0.165 [ 869] Vol = 566.0 Cell: 7.390 7.369 10.393 89.82 89.97 90.21 Volume: 566.04 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.403 ORTHORHOMBIC I-lattice R(int) = 0.117 [ 833] Vol = 566.0 Cell: 7.390 10.393 7.369 89.82 89.79 90.03 Volume: 566.04 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.253 MONOCLINIC I-lattice R(int) = 0.115 [ 680] Vol = 566.0 Cell: 10.393 7.390 7.369 90.21 90.18 90.03 Volume: 566.04 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.285 MONOCLINIC C-lattice R(int) = 0.107 [ 560] Vol = 566.0 Cell: 10.393 10.456 7.348 89.81 134.86 90.10 Volume: 566.04 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) = 0.055 [ 275] Vol = 283.0 Cell: 7.348 7.365 7.367 119.97 90.13 119.70 Volume: 283.02 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 0 721 0 958 954 1438 N (int>3sigma) = 0 0 0 0 105 0 208 212 302 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 25.8 25.5 24.4 Mean int/sigma = 0.0 0.0 0.0 0.0 1.8 0.0 4.8 4.5 4.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.112 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 10 10 119 258 N I>3s 0 0 1 62 0.1 0.1 -0.0 1.5 0.7 0.7 0.2 2.4 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 0.224 1113 Fd-3m 1 1 227 C N N N N 37 2284 0.223 1175 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.393493 10.456065 10.417150 89.8385 89.8529 90.1023 ZERR 1.00 0.009299 0.001631 0.017504 0.1881 0.0014 0.0040 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1187275- 116699 155 132 38 3.5 348137.22 31.68 0.109 0.097 113162- 2946 169 154 38 4.1 19227.96 5.20 0.203 0.142 2899- 1645 243 224 38 5.9 1856.15 2.18 0.751 0.775 1625- 1017 195 185 38 4.9 1150.60 1.39 0.654 0.715 1014- 808 171 163 38 4.3 829.36 1.22 0.597 0.671 806- 627 130 125 38 3.3 630.24 0.95 0.679 0.707 621- 450 142 139 38 3.7 488.48 0.92 0.697 0.764 449- 312 106 105 38 2.8 366.33 0.69 0.658 0.753 311- 106 124 120 38 3.2 185.46 0.54 0.788 1.262 104- -1002 92 91 41 2.2 13.64 0.23 0.979 2.650 ------------------------------------------------------------------------------------------- 1187275- -1002 1527 1438 383 3.8 34692.41 4.40 0.126 0.111 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-1.29 300 272 38 7.2 80831.04 9.10 0.122 0.106 0.027 1.26-0.98 249 234 38 6.2 45715.57 5.38 0.160 0.137 0.050 0.97-0.83 221 206 40 5.2 23483.12 3.41 0.075 0.064 0.063 0.82-0.75 167 159 38 4.2 30551.58 3.89 0.151 0.158 0.073 0.75-0.69 152 144 42 3.4 16944.06 2.56 0.099 0.072 0.091 0.69-0.64 139 134 41 3.3 15498.77 2.49 0.091 0.099 0.101 0.63-0.60 108 102 38 2.7 13327.79 2.21 0.131 0.134 0.114 0.60-0.56 87 83 38 2.2 9466.98 1.91 0.090 0.087 0.120 0.56-0.52 68 68 38 1.8 9524.50 1.96 0.089 0.102 0.129 0.52-0.46 36 36 32 1.1 5537.07 1.61 0.797 1.303 0.133 ------------------------------------------------------------------------------------------------------ inf-0.46 1527 1438 383 3.8 34692.41 4.40 0.126 0.111 0.052 inf-0.65 1195 1118 226 4.9 40973.92 5.02 0.128 0.110 0.046 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-1.29 272 38 38 100.0 7.2 80831.04 21.83 0.122 0.014 1.26-0.98 234 38 38 100.0 6.2 45715.57 11.86 0.160 0.027 0.97-0.83 206 40 40 100.0 5.2 23483.12 6.75 0.075 0.030 0.82-0.75 159 38 38 100.0 4.2 30551.58 7.65 0.151 0.043 0.75-0.69 144 42 42 100.0 3.4 16944.06 4.62 0.099 0.051 0.69-0.64 134 45 41 91.1 3.3 15498.77 4.29 0.091 0.060 0.63-0.60 102 41 38 92.7 2.7 13327.79 3.25 0.131 0.071 0.60-0.56 83 56 38 67.9 2.2 9466.98 2.59 0.090 0.076 0.56-0.52 68 79 38 48.1 1.8 9524.50 2.62 0.089 0.104 0.52-0.46 36 190 32 16.8 1.1 5537.07 1.59 0.797 1.637 -------------------------------------------------------------------------------------------- inf-0.46 1438 607 383 63.1 3.8 34692.41 9.28 0.126 0.032 inf-0.65 1118 229 226 98.7 4.9 40973.92 10.99 0.128 0.027 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.066514 0.012327 -0.008658 ( 0.000020 0.000026 0.000024 ) 0.014026 0.065130 -0.013489 ( 0.000019 0.000024 0.000022 ) 0.005979 -0.014697 -0.066146 ( 0.000029 0.000037 0.000034 ) M - matrix: 0.004657 0.000006 -0.000009 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004610 -0.000013 ( 0.000002 0.000004 0.000003 ) -0.000009 -0.000013 0.004632 ( 0.000002 0.000003 0.000004 ) Constraint UB - matrix: -0.066514 0.012327 -0.008658 ( 0.000020 0.000026 0.000024 ) 0.014026 0.065130 -0.013489 ( 0.000019 0.000024 0.000022 ) 0.005979 -0.014697 -0.066146 ( 0.000029 0.000037 0.000034 ) M - matrix: 0.004641 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004641 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004641 ( 0.000000 0.000000 0.000001 ) unit cell: 10.394(3) 10.447(4) 10.422(4) 89.84(3) 89.89(3) 90.07(3) V = 1131.7(8) unit cell: 10.4209(10) 10.4209(10) 10.4209(10) 90.0 90.0 90.0 V = 1131.67(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.114) Run 2 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.964) PROFFIT INFO: signal sum: min=-552.0000 max=8391635.0000 PROFFIT INFO: signal sum lp corr: min=-593.0519 max=1179168.2505 PROFFIT INFO: background sum: min=123.0000 max=8027.0000 PROFFIT INFO: background sum sig2: min=360.0000 max=5174.0000 PROFFIT INFO: num of signal pixels: min=36 max=515 PROFFIT INFO: Inet: min=-948.8831 max=1886669.2500 PROFFIT INFO: sig(Inet): min=64.7320 max=24238.9629 PROFFIT INFO: Inet/sig(Inet): min=-1.59 max=176.60 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 312 1082 1600 1910 2060 2386 2582 2700 2892 3028 3054 Percent 10.2 35.4 52.4 62.5 67.5 78.1 84.5 88.4 94.7 99.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1527 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 1527 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1886669- 126276 152 403356.66 76.31 100.00 125322- 4246 152 27684.28 19.13 100.00 4236- 2100 152 2904.22 7.21 100.00 2098- 1235 152 1604.41 3.79 50.66 1232- 806 152 1012.74 2.14 10.53 802- 554 152 676.17 1.68 7.24 553- 317 152 428.52 1.29 7.24 316- 128 152 215.94 0.60 0.66 128- 1 152 62.30 0.22 0.00 1- -949 159 -157.22 -0.30 0.00 ------------------------------------------------------------------------------------ 1886669- -949 1527 43577.39 11.16 37.46 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 152 97733.00 14.36 69.08 1.64- 1.26 152 84182.12 20.12 57.24 1.26- 1.06 152 61490.22 18.93 69.74 1.06- 0.95 152 56657.12 15.36 28.95 0.95- 0.88 152 29836.59 9.33 46.05 0.88- 0.81 152 38004.65 11.20 34.21 0.80- 0.75 152 20284.18 6.35 22.37 0.74- 0.71 152 23852.86 7.50 16.45 0.71- 0.67 152 22835.04 7.41 25.66 0.67- 0.63 159 2777.10 1.45 6.29 ------------------------------------------------------------------------------------ 6.00- 0.63 1527 43577.39 11.16 37.46 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:34:57 2019 Sorting 1527 observations 41 unique observations with > 7.00 F2/sig(F2) 1527 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 49 153 Total number of frames 153 Maximum number of 41 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1527 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 12 39 Total number of frames 39 365 observations > 7.00 F2/sig(F2) 365 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 12 39 Total number of frames 39 Removing 'redundancy=1' reflections Average redundancy: 8.0 (Out of 365 removed 7 = 358, unique = 45) 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 358 observations in 2 runs Run # start # end # total # 1 0 25 26 2 0 12 39 Total number of frames 39 45 unique data precomputed (should be 45) 45 unique data with 358 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.0 (Out of 358 removed 0 = 358, unique = 45) 45 unique data precomputed (should be 45) 45 unique data with 358 observations RMS deviation of equivalent data = 0.26484 Rint = 0.24126 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24126, wR= 0.31540 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09706, wR= 0.17828, Acormin=0.455, Acormax=1.260, Acor_av=0.867 F test: Probability=1.000, F= 6.080 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10532, wR= 0.16448, Acormin=0.349, Acormax=1.245, Acor_av=0.703 F test: Probability=0.000, F= 0.841 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11626, wR= 0.18688, Acormin=0.359, Acormax=1.444, Acor_av=0.742 F test: Probability=0.000, F= 0.677 Trying model 4 (ne=4, no=1)... Results: Rint= 0.11227, wR= 0.15332, Acormin=0.194, Acormax=1.276, Acor_av=0.644 F test: Probability=0.000, F= 0.718 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10623, wR= 0.15378, Acormin=0.045, Acormax=0.676, Acor_av=0.259 F test: Probability=0.000, F= 0.783 Final absorption model (ne=2, no=0): Rint= 0.09706, Acormin=0.455, Acormax=1.260, Acor_av=0.867 Combined refinement in use Rint: 0.24308 There are 39 active scales (one needs to be fixed) Refinement control: frame scale #38 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 43 pars with 946 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26484 Using Levenberg-Marquardt: 0.00010 New wR= 0.12043 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24126 with corrections 0.09444 Rint for all data: 0.24308 with corrections 0.09742 0 observations identified as outliers and rejected Cycle 2 wR= 0.12043 Using Levenberg-Marquardt: 0.00001 New wR= 0.10906 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24126 with corrections 0.08672 Rint for all data: 0.24308 with corrections 0.08980 0 observations identified as outliers and rejected Cycle 3 wR= 0.10906 Using Levenberg-Marquardt: 0.00000 New wR= 0.10801 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24126 with corrections 0.08770 Rint for all data: 0.24308 with corrections 0.09077 0 observations identified as outliers and rejected Cycle 4 wR= 0.10801 Using Levenberg-Marquardt: 0.00000 New wR= 0.10745 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24126 with corrections 0.08794 Rint for all data: 0.24308 with corrections 0.09101 0 observations identified as outliers and rejected Cycle 5 wR= 0.10745 Using Levenberg-Marquardt: 0.00000 New wR= 0.10700 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24126 with corrections 0.08802 Rint for all data: 0.24308 with corrections 0.09109 0 observations identified as outliers and rejected Final wR= 0.10700 Final frame scales: Min= 0.5956 Max= 1.4857 Final absorption correction factors: Amin= 0.5579 Amax= 1.3046 PROFFIT INFO: Inet (after scale3 abspack): min=-1072.0095 max=1304227.6250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=55.2241 max=22522.4648 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/103 1527 reflections read from tmp file 102 reflections are rejected (95 as outliers, 7 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 13 14 8 8 13 17 7 6 67 Initial Chi^2= 0.63730 Cycle 1, Chi^2= 1.08648 Current error model SIG(F2)^2 = 106.53*I_RAW + 0.95*I_BACK+(0.03501*)^2 Cycle 2, Chi^2= 1.00204 Current error model SIG(F2)^2 = 125.17*I_RAW + 1.37*I_BACK+(0.02200*)^2 Cycle 3, Chi^2= 0.99397 Current error model SIG(F2)^2 = 121.85*I_RAW + 1.81*I_BACK+(0.02408*)^2 Cycle 4, Chi^2= 1.00250 Current error model SIG(F2)^2 = 122.19*I_RAW + 1.61*I_BACK+(0.02353*)^2 Cycle 5, Chi^2= 0.99947 Current error model SIG(F2)^2 = 122.29*I_RAW + 1.65*I_BACK+(0.02364*)^2 Cycle 6, Chi^2= 1.00010 Current error model SIG(F2)^2 = 122.26*I_RAW + 1.64*I_BACK+(0.02362*)^2 Final Chi^2= 1.00010 Final error model SIG(F2)^2 = 122.26*I_RAW + 1.64*I_BACK+(0.02362*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1304228- 125259 152 374525.83 30.84 100.00 120736- 3667 152 28066.11 11.46 100.00 3660- 2040 152 2766.03 5.18 94.74 2034- 1149 152 1490.51 3.35 45.39 1146- 785 152 943.43 2.34 11.18 785- 531 152 661.55 2.08 9.87 528- 314 152 411.63 1.88 9.21 313- 133 152 212.14 1.26 1.32 133- 2 152 61.85 0.64 0.00 1- -1072 159 -159.32 -0.64 0.00 ------------------------------------------------------------------------------------ 1304228- -1072 1527 40709.76 5.81 37.00 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 152 89771.65 9.22 69.74 1.64- 1.26 152 78530.18 8.86 56.58 1.26- 1.06 152 60612.21 8.20 71.05 1.06- 0.95 152 53081.68 6.51 29.61 0.95- 0.88 152 25418.56 5.32 44.08 0.88- 0.81 152 37051.26 5.85 32.24 0.80- 0.75 152 19522.82 3.91 20.39 0.74- 0.71 152 20688.48 4.62 16.45 0.71- 0.67 152 21158.61 4.48 25.66 0.67- 0.63 159 2998.86 1.34 5.66 ------------------------------------------------------------------------------------ 6.00- 0.63 1527 40709.76 5.81 37.00 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 152 89771.65 9.22 69.74 6.00- 1.26 304 84150.91 9.04 63.16 6.00- 1.06 456 76304.68 8.76 65.79 6.00- 0.95 608 70498.93 8.20 56.74 6.00- 0.88 760 61482.86 7.62 54.21 6.00- 0.81 912 57410.92 7.33 50.55 6.00- 0.75 1064 51998.34 6.84 46.24 6.00- 0.71 1216 48084.60 6.56 42.52 6.00- 0.67 1368 45092.83 6.33 40.64 6.00- 0.63 1527 40709.76 5.81 37.00 ------------------------------------------------------------------------------------ 6.00- 0.63 1527 40709.76 5.81 37.00 Scale applied to data: s=0.766737 (maximum obs:1304227.625,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.091; Rsigma 0.038: data 1527 -> merged 161 With outlier rejection... Rint 0.066; Rsigma 0.040: data 1504 -> merged 161 Rejected total: 23, method kkm 19, method Blessing 4 Completeness direct cell (a, b, c) = (10.421, 10.421, 10.421), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627266, 6.016528 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.38 - 1.76 14 14 9.29 100.00 130 1.74 - 1.27 14 14 10.79 100.00 151 1.26 - 1.06 14 14 12.43 100.00 174 1.05 - 0.97 14 14 10.14 100.00 142 0.95 - 0.88 14 14 11.29 100.00 158 0.87 - 0.81 14 14 10.07 100.00 141 0.80 - 0.76 14 14 10.21 100.00 143 0.76 - 0.72 14 14 9.14 100.00 128 0.72 - 0.69 14 14 9.21 100.00 129 0.69 - 0.65 19 19 7.95 100.00 151 --------------------------------------------------------------- 7.38 - 0.65 145 145 9.98 100.00 1447 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:34:56 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.378044 7.364880 7.390205 120.2630 120.1524 89.6561 1438 Reflections read from file xs2212a.hkl 1438 Reflections used for space-group determination (up to diffraction limit of 0.59A); mean (I/sigma) = 4.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 738 733 721 728 1096 956 958 1438 N (int>3sigma) = 0 85 78 105 71 134 200 208 302 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.9 22.2 25.8 24.4 Mean int/sigma = 0.0 1.4 1.4 1.8 1.3 1.5 4.0 4.8 4.4 Lattice type: P chosen Volume: 283.02 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.348 7.365 7.367 119.97 90.13 119.70 Niggli form: a.a = 53.996 b.b = 54.241 c.c = 54.274 b.c = -27.104 a.c = -0.123 a.b = -26.811 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.498 CUBIC F-lattice R(int) = 0.225 [ 1204] Vol = 1132.1 Cell: 10.393 10.456 10.417 89.84 89.85 90.10 Volume: 1132.07 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.497 RHOMBOHEDRAL R-lattice R(int) = 0.209 [ 879] Vol = 849.1 Cell: 7.365 7.348 18.061 90.00 90.15 119.70 Volume: 849.06 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.497 RHOMBOHEDRAL R-lattice R(int) = 0.235 [ 269] Vol = 849.1 Trigonal Cell: 7.365 7.348 18.061 90.00 90.15 119.70 Volume: 849.06 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.538 TETRAGONAL I-lattice R(int) = 0.165 [ 869] Vol = 566.0 Cell: 7.390 7.369 10.393 89.82 89.97 90.21 Volume: 566.04 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.552 TETRAGONAL I-lattice R(int) = 0.165 [ 869] Vol = 566.0 Cell: 7.390 7.369 10.393 89.82 89.97 90.21 Volume: 566.04 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.403 ORTHORHOMBIC I-lattice R(int) = 0.117 [ 833] Vol = 566.0 Cell: 7.390 10.393 7.369 89.82 89.79 90.03 Volume: 566.04 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.253 MONOCLINIC I-lattice R(int) = 0.115 [ 680] Vol = 566.0 Cell: 10.393 7.390 7.369 90.21 90.18 90.03 Volume: 566.04 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.285 MONOCLINIC C-lattice R(int) = 0.107 [ 560] Vol = 566.0 Cell: 10.393 10.456 7.348 89.81 134.86 90.10 Volume: 566.04 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) = 0.055 [ 275] Vol = 283.0 Cell: 7.348 7.365 7.367 119.97 90.13 119.70 Volume: 283.02 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 0 721 0 958 954 1438 N (int>3sigma) = 0 0 0 0 105 0 208 212 302 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 25.8 25.5 24.4 Mean int/sigma = 0.0 0.0 0.0 0.0 1.8 0.0 4.8 4.5 4.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.112 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 10 10 119 258 N I>3s 0 0 1 62 0.1 0.1 -0.0 1.5 0.7 0.7 0.2 2.4 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 0.224 1113 Fd-3m 1 1 227 C N N N N 37 2284 0.223 1175 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.393493 10.456065 10.417150 89.8385 89.8529 90.1023 ZERR 1.00 0.009299 0.001631 0.017504 0.1881 0.0014 0.0040 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1160605- 99659 182 166 26 6.4 318893.92 28.52 0.062 0.058 85404- 2355 273 267 26 10.3 5505.07 7.16 0.110 0.098 1792- 809 294 293 26 11.3 1188.03 2.77 0.229 0.276 775- 374 284 284 26 10.9 550.85 1.89 0.394 0.500 368- 93 220 220 26 8.5 252.66 1.22 0.568 0.775 77- -323 274 274 31 8.8 -4.32 0.15 0.949 3.108 ------------------------------------------------------------------------------------------- 1160605- -323 1527 1504 161 9.3 36546.00 5.52 0.066 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-1.30 276 268 26 10.3 79752.32 9.11 0.060 0.052 0.029 1.27-1.00 288 286 26 11.0 56284.01 7.39 0.067 0.069 0.034 0.97-0.84 297 291 26 11.2 23422.02 4.75 0.053 0.049 0.050 0.82-0.74 254 250 26 9.6 16419.00 3.55 0.073 0.071 0.057 0.74-0.68 237 236 26 9.1 24286.08 5.06 0.091 0.105 0.061 0.68-0.63 175 173 31 5.6 4868.56 1.65 0.115 0.094 0.120 ------------------------------------------------------------------------------------------------------ inf-0.63 1527 1504 161 9.3 36546.00 5.52 0.066 0.061 0.040 inf-0.65 1467 1445 144 10.0 37842.36 5.69 0.066 0.061 0.039 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-1.30 268 26 26 100.0 10.3 79752.32 28.08 0.060 0.015 1.27-1.00 286 26 26 100.0 11.0 56284.01 24.14 0.067 0.013 0.97-0.84 291 26 26 100.0 11.2 23422.02 16.18 0.053 0.020 0.82-0.74 250 26 26 100.0 9.6 16419.00 9.91 0.073 0.022 0.74-0.68 236 26 26 100.0 9.1 24286.08 15.61 0.091 0.021 0.68-0.63 173 32 31 96.9 5.6 4868.56 3.86 0.115 0.052 -------------------------------------------------------------------------------------------- inf-0.63 1504 162 161 99.4 9.3 36546.00 17.27 0.066 0.017 inf-0.65 1445 144 144 100.0 10.0 37842.36 17.88 0.066 0.016 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:41:46 2019) ID: 3668; threads 40; handles 809; mem 515500.00 (1204688.00)kB; time: 1w 4d 22h 52m 33s MEMORY INFO: Memory PF:77.0, Ph:511.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.5,peak PF: 700.2, WS: 471.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:78.0, Ph:513.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.3,peak PF: 700.2, WS: 473.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:41:46 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000103 0.000065 0.000099 ) 0.064809 0.092374 0.027273 ( 0.000102 0.000065 0.000099 ) 0.045523 0.057900 0.132205 ( 0.000108 0.000068 0.000104 ) 7.38096 ( 0.00706 ) 7.36649 ( 0.00713 ) 7.42630 ( 0.00711 ) 120.52449 ( 0.10166 ) 120.40327 ( 0.10085 ) 89.27095 ( 0.07800 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:41:46 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000103 0.000065 0.000099 ) 0.064809 0.092374 0.027273 ( 0.000102 0.000065 0.000099 ) 0.045523 0.057900 0.132205 ( 0.000108 0.000068 0.000104 ) M - matrix: 0.013877 0.004573 0.009249 ( 0.000024 0.000014 0.000019 ) 0.004573 0.013976 0.009331 ( 0.000014 0.000016 0.000015 ) 0.009249 0.009331 0.018449 ( 0.000019 0.000015 0.000028 ) unit cell: 7.381(7) 7.366(7) 7.426(7) 120.52(10) 120.40(10) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb PROFFITPEAK info: 386 peaks in the peak location table UB fit with 44 obs out of 205 (total:205,skipped:0) (21.46%) UB - matrix: 0.085941 -0.047011 0.014980 ( 0.000732 0.000405 0.000827 ) 0.062958 0.092058 0.026253 ( 0.000676 0.000374 0.000763 ) 0.047009 0.058520 0.134321 ( 0.001019 0.000564 0.001151 ) M - matrix: 0.013559 0.004507 0.009254 ( 0.000180 0.000105 0.000172 ) 0.004507 0.014109 0.009573 ( 0.000105 0.000103 0.000130 ) 0.009254 0.009573 0.018956 ( 0.000172 0.000130 0.000313 ) unit cell: 7.46(5) 7.37(5) 7.36(7) 121.0(8) 120.3(8) 89.0(5) V = 283(4) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 205 #indexed refl 193, indexation with best UB: 94.1463% Lattice: 7.3841 7.3714 7.3445 120.236 120.046 89.627 282.390 Rotation: -23.948 24.224 -35.311 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 193 obs out of 205 (total:205,skipped:0) (94.15%) UB - matrix: 0.087434 -0.045151 0.014296 ( 0.000091 0.000094 0.000114 ) 0.061933 0.092752 0.025128 ( 0.000112 0.000115 0.000140 ) 0.048208 0.057118 0.133622 ( 0.000089 0.000092 0.000112 ) M - matrix: 0.013804 0.004550 0.009248 ( 0.000023 0.000017 0.000019 ) 0.004550 0.013904 0.009317 ( 0.000017 0.000025 0.000020 ) 0.009248 0.009317 0.018691 ( 0.000019 0.000020 0.000031 ) unit cell: 7.384(8) 7.371(9) 7.344(8) 120.24(13) 120.04(11) 89.63(9) V = 282.4(6) OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 UB fit with 193 obs out of 205 (total:205,skipped:0) (94.15%) UB - matrix: 0.087435 -0.045151 0.014296 ( 0.000091 0.000094 0.000114 ) 0.061933 0.092752 0.025128 ( 0.000112 0.000115 0.000140 ) 0.048208 0.057118 0.133622 ( 0.000089 0.000092 0.000112 ) M - matrix: 0.013804 0.004550 0.009248 ( 0.000023 0.000017 0.000019 ) 0.004550 0.013904 0.009317 ( 0.000017 0.000025 0.000020 ) 0.009248 0.009317 0.018691 ( 0.000019 0.000020 0.000031 ) unit cell: 7.384(8) 7.371(9) 7.344(8) 120.24(13) 120.04(11) 89.63(9) V = 282.4(6) OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 OTKP changes: 70 1 1 1 205 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Run 2 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1003 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087435 -0.045151 0.014296 ( 0.000091 0.000094 0.000114 ) 0.061933 0.092752 0.025128 ( 0.000112 0.000115 0.000140 ) 0.048208 0.057118 0.133622 ( 0.000089 0.000092 0.000112 ) M - matrix: 0.013804 0.004550 0.009248 ( 0.000023 0.000017 0.000019 ) 0.004550 0.013904 0.009317 ( 0.000017 0.000025 0.000020 ) 0.009248 0.009317 0.018691 ( 0.000019 0.000020 0.000031 ) UB fit with 193 obs out of 205 (total:205,skipped:0) (94.15%) unit cell: 7.384(8) 7.371(9) 7.344(8) 120.24(13) 120.04(11) 89.63(9) V = 282.4(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 193 obs out of 205 (total:205,skipped:0) (94.15%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb 0 of 186 peaks identified as outliers and rejected 186 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 186 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 186 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 19 | 0.857 ( 0.085) | 0.858 ( 0.127) | 1.047 ( 0.494) | 2.37- 1.76 | 19 | 0.877 ( 0.111) | 0.880 ( 0.169) | 0.945 ( 0.456) | 1.75- 1.58 | 19 | 0.902 ( 0.080) | 0.895 ( 0.139) | 0.966 ( 0.426) | 1.58- 1.35 | 19 | 0.938 ( 0.090) | 0.966 ( 0.127) | 0.948 ( 0.318) | 1.35- 1.19 | 19 | 0.938 ( 0.064) | 0.963 ( 0.091) | 0.995 ( 0.555) | 1.16- 1.08 | 19 | 0.902 ( 0.065) | 0.965 ( 0.143) | 0.787 ( 0.338) | 1.06- 0.89 | 19 | 0.956 ( 0.063) | 0.983 ( 0.098) | 1.095 ( 0.407) | 0.89- 0.82 | 19 | 0.944 ( 0.065) | 0.932 ( 0.085) | 1.132 ( 0.400) | 0.82- 0.72 | 19 | 0.931 ( 0.038) | 0.889 ( 0.093) | 1.391 ( 0.429) | 0.69- 0.63 | 15 | 0.922 ( 0.035) | 0.862 ( 0.062) | 1.453 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 186 | 0.916 ( 0.080) | 0.921 ( 0.127) | 1.068 ( 0.474) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 186 obs out of 186 (total:186,skipped:0) (100.00%) UB - matrix: 0.087476 -0.045185 0.014289 ( 0.000060 0.000063 0.000076 ) 0.062123 0.093125 0.025382 ( 0.000051 0.000054 0.000065 ) 0.048481 0.057157 0.133831 ( 0.000049 0.000051 0.000062 ) M - matrix: 0.013862 0.004604 0.009315 ( 0.000013 0.000009 0.000011 ) 0.004604 0.013981 0.009367 ( 0.000009 0.000013 0.000011 ) 0.009315 0.009367 0.018759 ( 0.000011 0.000011 0.000017 ) unit cell: 7.381(5) 7.354(5) 7.340(4) 120.19(6) 120.13(6) 89.70(5) V = 281.1(3) OTKP changes: 186 1 1 1 OTKP changes: 186 1 1 1 UB - matrix: 0.087464 -0.045169 0.014241 ( 0.000059 0.000063 0.000075 ) 0.062142 0.093050 0.025367 ( 0.000052 0.000056 0.000067 ) 0.048400 0.057176 0.133812 ( 0.000041 0.000043 0.000052 ) M - matrix: 0.013854 0.004599 0.009298 ( 0.000013 0.000009 0.000010 ) 0.004599 0.013968 0.009368 ( 0.000009 0.000013 0.000010 ) 0.009298 0.009368 0.018752 ( 0.000010 0.000010 0.000014 ) UB fit with 186 obs out of 186 (total:186,skipped:0) (100.00%) unit cell: 7.378(5) 7.360(5) 7.339(4) 120.23(6) 120.06(6) 89.71(5) V = 281.3(3) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.954) HKL list info: 1001 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087464 -0.045169 0.014241 ( 0.000059 0.000063 0.000075 ) 0.062142 0.093050 0.025367 ( 0.000052 0.000056 0.000067 ) 0.048400 0.057176 0.133812 ( 0.000041 0.000043 0.000052 ) M - matrix: 0.013854 0.004599 0.009298 ( 0.000013 0.000009 0.000010 ) 0.004599 0.013968 0.009368 ( 0.000009 0.000013 0.000010 ) 0.009298 0.009368 0.018752 ( 0.000010 0.000010 0.000014 ) UB fit with 186 obs out of 186 (total:186,skipped:0) (100.00%) unit cell: 7.378(5) 7.360(5) 7.339(4) 120.23(6) 120.06(6) 89.71(5) V = 281.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 186 obs out of 186 (total:186,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb 0 of 187 peaks identified as outliers and rejected 187 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 187 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 187 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 19 | 0.866 ( 0.084) | 0.864 ( 0.125) | 1.062 ( 0.493) | 2.37- 1.76 | 19 | 0.876 ( 0.099) | 0.880 ( 0.142) | 0.972 ( 0.502) | 1.75- 1.58 | 19 | 0.896 ( 0.091) | 0.894 ( 0.159) | 0.972 ( 0.453) | 1.58- 1.35 | 19 | 0.943 ( 0.093) | 0.974 ( 0.121) | 0.993 ( 0.477) | 1.35- 1.19 | 19 | 0.895 ( 0.071) | 0.919 ( 0.123) | 0.834 ( 0.425) | 1.19- 1.09 | 19 | 0.927 ( 0.074) | 0.959 ( 0.109) | 0.900 ( 0.408) | 1.09- 0.91 | 19 | 0.960 ( 0.070) | 0.979 ( 0.095) | 1.086 ( 0.432) | 0.89- 0.86 | 19 | 0.955 ( 0.064) | 0.913 ( 0.091) | 1.075 ( 0.380) | 0.82- 0.72 | 19 | 0.933 ( 0.038) | 0.901 ( 0.100) | 1.318 ( 0.403) | 0.72- 0.63 | 16 | 0.924 ( 0.035) | 0.861 ( 0.063) | 1.496 ( 0.487) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 187 | 0.917 ( 0.082) | 0.915 ( 0.123) | 1.064 ( 0.483) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-11.4 | 40 | 0.975 ( 0.039) | 1.021 ( 0.081) | 1.143 ( 0.471) | 11.6-15.8 | 40 | 1.031 ( 0.320) | 1.063 ( 0.095) | 1.389 ( 1.621) | 15.9-20.1 | 40 | 0.952 ( 0.059) | 1.009 ( 0.094) | 1.040 ( 0.476) | 20.5-24.2 | 40 | 0.951 ( 0.054) | 0.999 ( 0.085) | 0.927 ( 0.411) | 24.2-27.6 | 40 | 0.950 ( 0.073) | 0.986 ( 0.115) | 1.004 ( 0.441) | 28.0-32.9 | 40 | 0.929 ( 0.105) | 0.932 ( 0.113) | 0.954 ( 0.491) | 33.1-36.7 | 40 | 0.917 ( 0.223) | 0.877 ( 0.121) | 1.124 ( 0.806) | 36.9-39.1 | 40 | 0.855 ( 0.082) | 0.830 ( 0.125) | 1.045 ( 0.527) | 39.1-42.0 | 40 | 0.887 ( 0.091) | 0.832 ( 0.130) | 1.150 ( 0.509) | 42.0-49.8 | 39 | 0.854 ( 0.109) | 0.768 ( 0.112) | 1.076 ( 0.538) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 399 | 0.930 ( 0.152) | 0.932 ( 0.144) | 1.085 ( 0.729) | Fitted profile normalization line parameters e1 dimension: a=-0.0037 b=1.14 e2 dimension: a=-0.0081 b=1.28 e3 dimension: a=0.0061 b=0.90 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5551 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386532 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1337741 PROFFITPEAK - Finished at Wed Aug 21 12:41:53 2019 PROFFITMAIN - Started at Wed Aug 21 12:41:53 2019 OTKP changes: 241 2 1 2 OTKP changes: 241 2 1 2 OTKP changes: 241 2 1 2 UB - matrix: 0.087480 -0.046061 0.017157 ( 0.000098 0.000062 0.000095 ) 0.064298 0.092381 0.027220 ( 0.000097 0.000062 0.000095 ) 0.045483 0.057670 0.131984 ( 0.000107 0.000068 0.000104 ) M - matrix: 0.013856 0.004534 0.009254 ( 0.000023 0.000014 0.000018 ) 0.004534 0.013982 0.009336 ( 0.000014 0.000015 0.000015 ) 0.009254 0.009336 0.018455 ( 0.000018 0.000015 0.000028 ) UB fit with 249 obs out of 399 (total:399,skipped:0) (62.41%) unit cell: 7.390(7) 7.372(7) 7.439(7) 120.62(10) 120.41(10) 89.08(7) V = 284.4(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 202 obs out of 212 (total:212,skipped:0) (95.28%) UB - matrix: 0.087484 -0.046132 0.017405 ( 0.000099 0.000061 0.000092 ) 0.064743 0.092333 0.027257 ( 0.000087 0.000054 0.000080 ) 0.045692 0.057798 0.132110 ( 0.000105 0.000065 0.000097 ) M - matrix: 0.013933 0.004583 0.009324 ( 0.000023 0.000013 0.000018 ) 0.004583 0.013994 0.009349 ( 0.000013 0.000014 0.000013 ) 0.009324 0.009349 0.018499 ( 0.000018 0.000013 0.000026 ) unit cell: 7.382(6) 7.368(6) 7.436(6) 120.52(9) 120.49(9) 89.20(7) V = 283.6(4) OTKP changes: 199 1 1 1 OTKP changes: 199 1 1 1 OTKP changes: 199 1 1 1 UB - matrix: 0.087335 -0.045927 0.017472 ( 0.000098 0.000061 0.000092 ) 0.064635 0.092275 0.027275 ( 0.000086 0.000053 0.000081 ) 0.045504 0.057766 0.131952 ( 0.000102 0.000063 0.000096 ) M - matrix: 0.013876 0.004582 0.009293 ( 0.000022 0.000013 0.000017 ) 0.004582 0.013961 0.009337 ( 0.000013 0.000013 0.000013 ) 0.009293 0.009337 0.018461 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.397(6) 7.380(6) 7.444(6) 120.52(9) 120.44(9) 89.26(7) V = 285.0(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087334 -0.045926 0.017472 ( 0.000098 0.000061 0.000092 ) 0.064635 0.092275 0.027275 ( 0.000086 0.000053 0.000081 ) 0.045503 0.057766 0.131952 ( 0.000102 0.000063 0.000096 ) M - matrix: 0.013875 0.004582 0.009293 ( 0.000022 0.000013 0.000017 ) 0.004582 0.013961 0.009337 ( 0.000013 0.000013 0.000013 ) 0.009293 0.009337 0.018461 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.397(6) 7.380(6) 7.444(6) 120.52(9) 120.44(9) 89.26(7) V = 285.0(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.117988 0.039076 0.078750 ( 0.000075 0.000047 0.000069 ) 0.000037 0.111466 0.056200 ( 0.000075 0.000047 0.000070 ) 0.000026 -0.000046 0.095444 ( 0.000090 0.000056 0.000083 ) M - matrix: 0.013921 0.004615 0.009296 ( 0.000018 0.000010 0.000014 ) 0.004615 0.013952 0.009337 ( 0.000010 0.000011 0.000011 ) 0.009296 0.009337 0.018470 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.378(5) 7.383(5) 7.431(8) 120.46(9) 120.29(9) 89.47(5) V = 284.3(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 187 obs out of 187 (total:187,skipped:0) (100.00%) UB - matrix: 0.087455 -0.045173 0.014258 ( 0.000059 0.000063 0.000075 ) 0.062195 0.093111 0.025418 ( 0.000052 0.000055 0.000065 ) 0.048375 0.057155 0.133804 ( 0.000040 0.000043 0.000051 ) M - matrix: 0.013857 0.004605 0.009301 ( 0.000013 0.000009 0.000010 ) 0.004605 0.013977 0.009370 ( 0.000009 0.000013 0.000010 ) 0.009301 0.009370 0.018753 ( 0.000010 0.000010 0.000014 ) unit cell: 7.377(5) 7.357(5) 7.338(4) 120.21(6) 120.06(6) 89.74(5) V = 281.1(3) OTKP changes: 187 1 1 1 OTKP changes: 187 1 1 1 UB - matrix: 0.087432 -0.045178 0.014246 ( 0.000060 0.000063 0.000075 ) 0.062191 0.093071 0.025426 ( 0.000052 0.000055 0.000066 ) 0.048342 0.057144 0.133767 ( 0.000040 0.000042 0.000050 ) M - matrix: 0.013849 0.004601 0.009293 ( 0.000013 0.000009 0.000010 ) 0.004601 0.013969 0.009367 ( 0.000009 0.000013 0.000010 ) 0.009293 0.009367 0.018743 ( 0.000010 0.000010 0.000014 ) UB fit with 187 obs out of 187 (total:187,skipped:0) (100.00%) unit cell: 7.379(5) 7.360(5) 7.341(4) 120.23(6) 120.05(6) 89.73(5) V = 281.4(3) Run 2 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.966) HKL list info: 993 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087432 -0.045178 0.014246 ( 0.000060 0.000063 0.000075 ) 0.062191 0.093071 0.025426 ( 0.000052 0.000055 0.000066 ) 0.048342 0.057144 0.133767 ( 0.000040 0.000042 0.000050 ) M - matrix: 0.013849 0.004601 0.009293 ( 0.000013 0.000009 0.000010 ) 0.004601 0.013969 0.009367 ( 0.000009 0.000013 0.000010 ) 0.009293 0.009367 0.018743 ( 0.000010 0.000010 0.000014 ) UB fit with 187 obs out of 187 (total:187,skipped:0) (100.00%) unit cell: 7.379(5) 7.360(5) 7.341(4) 120.23(6) 120.05(6) 89.73(5) V = 281.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 187 obs out of 187 (total:187,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117825 0.039238 0.079041 ( 0.000049 0.000052 0.000062 ) 0.000037 0.111557 0.056284 ( 0.000051 0.000054 0.000064 ) 0.000012 0.000014 0.096602 ( 0.000040 0.000043 0.000051 ) M - matrix: 0.013883 0.004627 0.009316 ( 0.000011 0.000009 0.000010 ) 0.004627 0.013985 0.009382 ( 0.000009 0.000013 0.000010 ) 0.009316 0.009382 0.018747 ( 0.000010 0.000010 0.000016 ) UB fit with 187 obs out of 187 (total:187,skipped:0) (100.00%) unit cell: 7.374(4) 7.359(4) 7.343(4) 120.22(6) 120.06(6) 89.79(4) V = 281.1(2) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117805 0.039061 0.078776 ( 0.000045 0.000035 0.000046 ) -0.000020 0.111479 0.056180 ( 0.000044 0.000034 0.000045 ) -0.000032 -0.000196 0.095917 ( 0.000061 0.000047 0.000062 ) M - matrix: 0.013878 0.004599 0.009276 ( 0.000011 0.000007 0.000009 ) 0.004599 0.013953 0.009321 ( 0.000007 0.000008 0.000008 ) 0.009276 0.009321 0.018562 ( 0.000009 0.000008 0.000015 ) UB fit with 393 obs out of 399 (total:399,skipped:0) (98.50%) unit cell: 7.378(3) 7.366(3) 7.386(6) 120.26(6) 120.16(6) 89.64(4) V = 282.9(3) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 57 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof 1774 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:41:56 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.966) PROFFIT INFO: signal sum: min=-574.0000 max=7870996.0000 PROFFIT INFO: signal sum lp corr: min=-592.8123 max=1101299.6594 PROFFIT INFO: background sum: min=134.0000 max=7337.0000 PROFFIT INFO: background sum sig2: min=411.0000 max=5075.0000 PROFFIT INFO: num of signal pixels: min=38 max=505 PROFFIT INFO: Inet: min=-948.4997 max=1762079.3750 PROFFIT INFO: sig(Inet): min=64.7799 max=24173.8242 PROFFIT INFO: Inet/sig(Inet): min=-1.65 max=180.81 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 176 633 930 1113 1203 1384 1500 1566 1681 1758 1774 Percent 9.9 35.7 52.4 62.7 67.8 78.0 84.6 88.3 94.8 99.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1774 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 1774 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1762079- 128554 177 403740.16 75.90 100.00 128239- 4126 177 28277.07 19.08 100.00 4040- 2014 177 2816.87 7.00 97.74 2010- 1211 177 1553.93 3.73 50.28 1209- 799 177 994.94 2.21 10.17 797- 533 177 667.59 1.65 7.91 531- 314 177 418.73 1.27 6.78 313- 130 177 209.22 0.61 0.56 130- 3 177 64.12 0.23 0.00 2- -948 181 -145.49 -0.28 0.00 ------------------------------------------------------------------------------------ 1762079- -948 1774 43760.49 11.11 37.26 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 177 100571.60 15.62 68.93 1.64- 1.26 177 88646.86 20.66 57.06 1.26- 1.04 177 56867.99 15.60 50.85 1.04- 0.92 177 21784.75 7.70 38.42 0.92- 0.83 177 48019.55 13.70 33.90 0.83- 0.76 177 27679.18 8.90 31.64 0.75- 0.69 177 41209.16 11.79 35.59 0.69- 0.64 177 23332.34 7.13 21.47 0.64- 0.58 177 13281.87 4.70 19.21 0.58- 0.46 181 16820.42 5.47 16.02 ------------------------------------------------------------------------------------ 6.55- 0.46 1774 43760.49 11.11 37.26 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:41:56 2019 Sorting 1774 observations 73 unique observations with > 7.00 F2/sig(F2) 1774 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 74 178 Total number of frames 178 Maximum number of 73 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1774 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 24 60 Total number of frames 60 422 observations > 7.00 F2/sig(F2) 422 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 24 60 Total number of frames 60 Removing 'redundancy=1' reflections Average redundancy: 4.2 (Out of 422 removed 39 = 383, unique = 91) 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 383 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 24 60 Total number of frames 60 91 unique data precomputed (should be 91) 91 unique data with 383 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.2 (Out of 383 removed 0 = 383, unique = 91) 91 unique data precomputed (should be 91) 91 unique data with 383 observations RMS deviation of equivalent data = 0.38685 Rint = 0.36157 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.36157, wR= 0.49437 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26239, wR= 0.35141, Acormin=0.238, Acormax=1.421, Acor_av=0.754 F test: Probability=1.000, F= 1.866 Trying model 2 (ne=2, no=1)... Results: Rint= 0.29864, wR= 0.36825, Acormin=0.108, Acormax=1.504, Acor_av=0.533 F test: Probability=0.000, F= 0.764 Trying model 3 (ne=4, no=0)... Results: Rint= 0.28934, wR= 0.33821, Acormin=0.075, Acormax=1.631, Acor_av=0.565 F test: Probability=0.000, F= 0.797 Trying model 4 (ne=4, no=1)... Results: Rint= 0.30680, wR= 0.35149, Acormin=0.057, Acormax=1.344, Acor_av=0.463 F test: Probability=0.000, F= 0.701 Trying model 5 (ne=4, no=3)... Results: Rint= 0.46231, wR= 0.39734, Acormin=-0.117, Acormax=0.856, Acor_av=0.195 F test: Probability=0.000, F= 0.301 Trying model 6 (ne=6, no=0)... Results: Rint= 0.31425, wR= 0.36885, Acormin=-0.065, Acormax=2.007, Acor_av=0.341 F test: Probability=0.000, F= 0.644 Trying model 7 (ne=6, no=1)... Results: Rint= 0.35758, wR= 0.39040, Acormin=-0.012, Acormax=1.754, Acor_av=0.311 F test: Probability=0.000, F= 0.492 Trying model 8 (ne=6, no=3)... Results: Rint= 0.38803, wR= 0.34042, Acormin=-0.141, Acormax=1.280, Acor_av=0.203 F test: Probability=0.000, F= 0.406 Trying model 9 (ne=6, no=5)... Results: Rint= 0.34492, wR= 0.33667, Acormin=-0.083, Acormax=0.704, Acor_av=0.070 F test: Probability=0.000, F= 0.492 Trying model 10 (ne=8, no=0)... Results: Rint= 0.37242, wR= 0.41693, Acormin=-0.054, Acormax=1.667, Acor_av=0.201 F test: Probability=0.000, F= 0.429 Trying model 11 (ne=8, no=1)... Results: Rint= 0.44073, wR= 0.46293, Acormin=-0.124, Acormax=1.311, Acor_av=0.153 F test: Probability=0.000, F= 0.303 Trying model 12 (ne=8, no=3)... Results: Rint= 0.19558, wR= 0.22605, Acormin=-0.008, Acormax=0.179, Acor_av=0.056 F test: Probability=0.999, F= 1.493 Trying model 13 (ne=8, no=5)... Results: Rint= 0.17437, wR= 0.19365, Acormin=-0.003, Acormax=0.186, Acor_av=0.064 F test: Probability=1.000, F= 1.791 Trying model 14 (ne=8, no=7)... Results: Rint= 0.12431, wR= 0.16641, Acormin=0.011, Acormax=0.288, Acor_av=0.078 F test: Probability=1.000, F= 3.291 Final absorption model (ne=2, no=0): Rint= 0.26239, Acormin=0.238, Acormax=1.421, Acor_av=0.754 Combined refinement in use Rint: 0.37540 There are 60 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 64 pars with 2080 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.38685 Using Levenberg-Marquardt: 0.00010 New wR= 0.19568 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.36157 with corrections 0.16239 Rint for all data: 0.37540 with corrections 0.17854 0 observations identified as outliers and rejected Cycle 2 wR= 0.19568 Using Levenberg-Marquardt: 0.00001 New wR= 0.18631 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.36157 with corrections 0.15430 Rint for all data: 0.37540 with corrections 0.17074 0 observations identified as outliers and rejected Cycle 3 wR= 0.18631 Using Levenberg-Marquardt: 0.00000 New wR= 0.18439 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.36157 with corrections 0.15495 Rint for all data: 0.37540 with corrections 0.17140 0 observations identified as outliers and rejected Cycle 4 wR= 0.18439 Using Levenberg-Marquardt: 0.00000 New wR= 0.18408 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.36157 with corrections 0.15557 Rint for all data: 0.37540 with corrections 0.17199 0 observations identified as outliers and rejected Cycle 5 wR= 0.18408 Using Levenberg-Marquardt: 0.00000 New wR= 0.18355 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.36157 with corrections 0.15544 Rint for all data: 0.37540 with corrections 0.17186 0 observations identified as outliers and rejected Final wR= 0.18355 Final frame scales: Min= 0.6021 Max= 1.8773 Final absorption correction factors: Amin= 0.4178 Amax= 1.3770 PROFFIT INFO: Inet (after scale3 abspack): min=-1677.6772 max=1433618.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=41.3609 max=24279.9160 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/103 1774 reflections read from tmp file 476 reflections are rejected (399 as outliers, 77 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 70 73 47 30 36 31 10 1 7 Initial Chi^2= 2.59153 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.78522 Current error model SIG(F2)^2 = 567.13*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 445.32*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 445.32*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1433619- 123953 177 358121.79 30.97 100.00 123683- 3879 177 25595.39 6.46 83.05 3869- 1878 177 2569.89 2.57 23.73 1872- 1106 177 1444.43 1.80 11.86 1105- 743 177 913.75 1.40 3.95 742- 468 177 602.05 1.05 0.56 468- 275 177 368.83 1.00 0.00 274- 122 177 192.85 0.80 2.26 122- 3 177 58.80 0.40 0.00 2- -1678 181 -178.39 -0.35 0.00 ------------------------------------------------------------------------------------ 1433619- -1678 1774 38880.67 4.60 22.49 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 177 93848.48 10.58 48.59 1.64- 1.26 177 83729.49 8.44 39.55 1.26- 1.04 177 52982.88 6.00 32.20 1.04- 0.92 177 23420.42 2.84 13.56 0.92- 0.83 177 38498.17 4.62 19.21 0.83- 0.76 177 25111.78 3.14 15.82 0.75- 0.69 177 32467.19 4.02 19.77 0.69- 0.64 177 17979.61 2.60 14.69 0.64- 0.58 177 10677.64 1.78 9.60 0.58- 0.46 181 10727.27 2.02 12.15 ------------------------------------------------------------------------------------ 6.55- 0.46 1774 38880.67 4.60 22.49 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 177 93848.48 10.58 48.59 6.55- 1.26 354 88788.98 9.51 44.07 6.55- 1.04 531 76853.62 8.34 40.11 6.55- 0.92 708 63495.32 6.96 33.47 6.55- 0.83 885 58495.89 6.50 30.62 6.55- 0.76 1062 52931.87 5.94 28.15 6.55- 0.69 1239 50008.35 5.66 26.96 6.55- 0.64 1416 46004.75 5.28 25.42 6.55- 0.58 1593 42079.52 4.89 23.67 6.55- 0.46 1774 38880.67 4.60 22.49 ------------------------------------------------------------------------------------ 6.55- 0.46 1774 38880.67 4.60 22.49 Scale applied to data: s=0.697535 (maximum obs:1433618.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.172; Rsigma 0.052: data 1774 -> merged 388 With outlier rejection... Rint 0.118; Rsigma 0.055: data 1672 -> merged 388 Rejected total: 102, method kkm 98, method Blessing 4 Completeness direct cell (a, b, c) = (6.565, 6.565, 6.565), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.457401, 6.564937 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.59 22 22 8.32 100.00 183 1.55 - 1.22 22 22 7.73 100.00 170 1.20 - 1.03 22 22 7.05 100.00 155 1.03 - 0.92 22 22 6.32 100.00 139 0.92 - 0.84 22 22 6.18 100.00 136 0.84 - 0.79 22 22 4.91 100.00 108 0.79 - 0.75 22 22 5.36 100.00 118 0.75 - 0.71 22 22 3.91 100.00 86 0.71 - 0.69 22 22 4.09 100.00 90 0.68 - 0.65 28 31 4.18 90.32 117 --------------------------------------------------------------- 7.37 - 0.65 226 229 5.76 98.69 1302 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:41:57 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.378109 7.366083 7.386091 120.2632 120.1569 89.6364 1672 Reflections read from file xs2212a.hkl 1672 Reflections used for space-group determination (up to diffraction limit of 0.60A); mean (I/sigma) = 4.10 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 860 847 843 847 1275 1108 1106 1672 N (int>3sigma) = 0 87 83 114 74 142 220 224 332 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.8 20.7 24.1 23.0 Mean int/sigma = 0.0 1.3 1.3 1.7 1.2 1.4 3.8 4.4 4.1 Lattice type: P chosen Volume: 282.94 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.347 7.365 7.366 119.94 119.73 90.11 Niggli form: a.a = 53.975 b.b = 54.237 c.c = 54.259 b.c = -27.075 a.c = -26.840 a.b = -0.103 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.509 CUBIC F-lattice R(int) = 0.213 [ 1437] Vol = 1131.8 Cell: 10.459 10.412 10.393 89.86 90.09 89.89 Volume: 1131.75 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.422 TETRAGONAL I-lattice R(int) = 0.163 [ 1094] Vol = 565.9 Cell: 7.372 7.386 10.393 90.03 89.84 89.75 Volume: 565.88 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.330 TETRAGONAL I-lattice R(int) = 0.192 [ 1089] Vol = 565.9 Cell: 7.347 7.365 10.459 90.01 89.86 90.11 Volume: 565.88 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.263 TETRAGONAL I-lattice R(int) = 0.163 [ 1094] Vol = 565.9 Cell: 7.386 7.372 10.393 90.16 90.03 90.25 Volume: 565.88 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.351 ORTHORHOMBIC F-lattice R(int) = 0.156 [ 1074] Vol = 1131.8 Cell: 10.393 10.412 10.459 89.89 90.09 89.86 Volume: 1131.75 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.448 ORTHORHOMBIC I-lattice R(int) = 0.119 [ 1051] Vol = 565.9 Cell: 10.393 7.386 7.372 89.75 89.84 90.03 Volume: 565.88 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.185 ORTHORHOMBIC I-lattice R(int) = 0.189 [ 1051] Vol = 565.9 Cell: 7.347 7.365 10.459 89.99 90.14 90.11 Volume: 565.88 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.311 MONOCLINIC I-lattice R(int) = 0.075 [ 676] Vol = 565.9 Cell: 7.372 10.393 7.386 90.03 90.25 90.16 Volume: 565.88 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.319 MONOCLINIC I-lattice R(int) = 0.155 [ 793] Vol = 565.9 Cell: 7.366 10.412 7.378 89.98 90.36 89.82 Volume: 565.88 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.272 MONOCLINIC I-lattice R(int) = 0.075 [ 676] Vol = 565.9 Cell: 7.386 10.393 7.372 90.16 90.25 90.03 Volume: 565.88 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.112 MONOCLINIC I-lattice R(int) = 0.177 [ 750] Vol = 565.9 Cell: 7.347 7.365 10.459 90.01 90.14 89.89 Volume: 565.88 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.096 MONOCLINIC I-lattice R(int) = 0.130 [ 691] Vol = 565.9 Cell: 7.347 10.459 7.365 90.01 90.11 89.86 Volume: 565.88 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.235 MONOCLINIC I-lattice R(int) = 0.130 [ 691] Vol = 565.9 Cell: 7.347 10.459 7.365 89.99 90.11 90.14 Volume: 565.88 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.067 [ 309] Vol = 282.9 Cell: 7.347 7.365 7.366 119.94 119.73 90.11 Volume: 282.94 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 0 843 0 1110 1113 1672 N (int>3sigma) = 0 0 0 0 114 0 233 232 332 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 24.6 22.6 23.0 Mean int/sigma = 0.0 0.0 0.0 0.0 1.7 0.0 4.2 4.1 4.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.982 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 10 10 133 302 N I>3s 0 0 0 68 0.1 0.1 -0.0 1.4 0.7 0.7 0.1 2.2 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 0.213 1332 Fd-3m 1 1 227 C N N N N 37 2284 0.214 1394 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.458750 10.412385 10.392588 89.8610 90.0935 89.8911 ZERR 1.00 0.001429 0.015359 0.008170 0.0006 0.0018 0.1644 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 976440- 128650 181 152 38 4.0 334512.95 29.67 0.100 0.086 121699- 2990 188 172 38 4.5 18950.89 4.81 0.203 0.131 2988- 1573 293 272 38 7.2 1798.81 2.13 0.761 0.815 1549- 1072 203 189 38 5.0 1116.13 1.29 0.631 0.687 1070- 844 204 198 38 5.2 849.41 1.15 0.713 0.755 842- 629 158 153 38 4.0 653.90 1.00 0.682 0.751 629- 490 166 161 38 4.2 506.97 0.79 0.753 0.841 488- 372 132 131 38 3.4 410.93 0.75 0.618 0.731 364- 180 117 114 38 3.0 271.57 0.57 0.749 0.904 179- -1045 132 130 46 2.8 52.15 0.23 0.919 2.178 ------------------------------------------------------------------------------------------- 976440- -1045 1774 1672 388 4.3 33042.56 4.10 0.118 0.100 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-1.29 343 311 38 8.2 78482.49 8.77 0.113 0.080 0.028 1.26-0.98 289 268 38 7.1 37581.46 4.51 0.133 0.121 0.054 0.97-0.83 240 229 38 6.0 27136.52 3.66 0.089 0.068 0.065 0.83-0.75 197 187 38 4.9 29600.67 3.59 0.176 0.192 0.075 0.75-0.70 168 158 38 4.2 18592.58 2.54 0.084 0.074 0.096 0.69-0.64 169 161 39 4.1 16822.17 2.42 0.095 0.092 0.102 0.64-0.61 124 120 38 3.2 8497.98 1.46 0.127 0.112 0.150 0.61-0.57 112 107 38 2.8 11519.35 1.96 0.124 0.131 0.125 0.57-0.54 77 76 38 2.0 9155.30 1.93 0.077 0.074 0.128 0.53-0.46 55 55 45 1.2 7701.24 1.67 0.465 0.474 0.141 ------------------------------------------------------------------------------------------------------ inf-0.46 1774 1672 388 4.3 33042.56 4.10 0.118 0.100 0.055 inf-0.65 1392 1302 226 5.8 38686.48 4.67 0.118 0.098 0.049 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-1.29 311 38 38 100.0 8.2 78482.49 22.51 0.113 0.013 1.26-0.98 268 38 38 100.0 7.1 37581.46 9.97 0.133 0.027 0.97-0.83 229 38 38 100.0 6.0 27136.52 8.01 0.089 0.030 0.83-0.75 187 38 38 100.0 4.9 29600.67 7.76 0.176 0.042 0.75-0.70 158 38 38 100.0 4.2 18592.58 5.06 0.084 0.048 0.69-0.64 161 43 39 90.7 4.1 16822.17 4.84 0.095 0.054 0.64-0.61 120 41 38 92.7 3.2 8497.98 2.45 0.127 0.083 0.61-0.57 107 53 38 71.7 2.8 11519.35 3.07 0.124 0.075 0.57-0.54 76 66 38 57.6 2.0 9155.30 2.68 0.077 0.091 0.53-0.46 55 219 45 20.5 1.2 7701.24 1.68 0.465 1.081 -------------------------------------------------------------------------------------------- inf-0.46 1672 613 388 63.3 4.3 33042.56 9.24 0.118 0.032 inf-0.65 1302 229 226 98.7 5.8 38686.48 10.89 0.118 0.026 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 No constraint UB - matrix: 0.012426 -0.008701 -0.066487 ( 0.000023 0.000020 0.000017 ) 0.065078 -0.013464 0.014139 ( 0.000022 0.000020 0.000016 ) -0.014761 -0.066194 0.005992 ( 0.000034 0.000030 0.000025 ) M - matrix: 0.004607 -0.000007 0.000005 ( 0.000004 0.000003 0.000002 ) -0.000007 0.004639 -0.000008 ( 0.000003 0.000003 0.000002 ) 0.000005 -0.000008 0.004656 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.012426 -0.008701 -0.066487 ( 0.000023 0.000020 0.000017 ) 0.065078 -0.013464 0.014139 ( 0.000022 0.000020 0.000016 ) -0.014761 -0.066194 0.005992 ( 0.000034 0.000030 0.000025 ) M - matrix: 0.004641 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004641 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004641 ( 0.000000 0.000000 0.000001 ) unit cell: 10.450(4) 10.414(4) 10.395(3) 89.90(3) 90.07(3) 89.91(3) V = 1131.2(7) unit cell: 10.4196(9) 10.4196(9) 10.4196(9) 90.0 90.0 90.0 V = 1131.22(18) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=52.966) PROFFIT INFO: signal sum: min=-574.0000 max=7870996.0000 PROFFIT INFO: signal sum lp corr: min=-592.8123 max=1101299.6594 PROFFIT INFO: background sum: min=134.0000 max=7337.0000 PROFFIT INFO: background sum sig2: min=411.0000 max=5075.0000 PROFFIT INFO: num of signal pixels: min=38 max=505 PROFFIT INFO: Inet: min=-948.4997 max=1762079.3750 PROFFIT INFO: sig(Inet): min=64.7799 max=24173.8242 PROFFIT INFO: Inet/sig(Inet): min=-1.65 max=180.81 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 352 1266 1860 2226 2406 2768 3000 3132 3362 3516 3548 Percent 9.9 35.7 52.4 62.7 67.8 78.0 84.6 88.3 94.8 99.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1774 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 1774 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1762079- 128554 177 403740.16 75.90 100.00 128239- 4126 177 28277.07 19.08 100.00 4040- 2014 177 2816.87 7.00 97.74 2010- 1211 177 1553.93 3.73 50.28 1209- 799 177 994.94 2.21 10.17 797- 533 177 667.59 1.65 7.91 531- 314 177 418.73 1.27 6.78 313- 130 177 209.22 0.61 0.56 130- 3 177 64.12 0.23 0.00 2- -948 181 -145.49 -0.28 0.00 ------------------------------------------------------------------------------------ 1762079- -948 1774 43760.49 11.11 37.26 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 177 108096.46 14.51 69.49 1.64- 1.26 177 79312.09 20.15 57.63 1.26- 1.09 177 58992.32 18.17 66.10 1.09- 0.97 177 55527.20 15.40 31.07 0.97- 0.88 177 21462.75 7.55 42.37 0.88- 0.81 177 46564.27 13.16 36.72 0.80- 0.76 177 17902.92 5.70 21.47 0.75- 0.71 177 24726.31 7.74 17.51 0.71- 0.67 177 22989.81 7.43 24.86 0.67- 0.63 181 2952.97 1.54 6.08 ------------------------------------------------------------------------------------ 6.00- 0.63 1774 43760.49 11.11 37.26 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:41:57 2019 Sorting 1774 observations 41 unique observations with > 7.00 F2/sig(F2) 1774 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 74 178 Total number of frames 178 Maximum number of 41 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 1774 observations in 2 runs Run # start # end # total # 1 0 20 21 2 0 14 36 Total number of frames 36 422 observations > 7.00 F2/sig(F2) 422 observations in 2 runs Run # start # end # total # 1 0 20 21 2 0 14 36 Total number of frames 36 Removing 'redundancy=1' reflections Average redundancy: 9.2 (Out of 422 removed 8 = 414, unique = 45) 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 414 observations in 2 runs Run # start # end # total # 1 0 20 21 2 0 14 36 Total number of frames 36 45 unique data precomputed (should be 45) 45 unique data with 414 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 9.2 (Out of 414 removed 0 = 414, unique = 45) 45 unique data precomputed (should be 45) 45 unique data with 414 observations RMS deviation of equivalent data = 0.24962 Rint = 0.21493 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.21493, wR= 0.28903 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09533, wR= 0.17258, Acormin=0.564, Acormax=1.236, Acor_av=0.949 F test: Probability=1.000, F= 5.014 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10051, wR= 0.15528, Acormin=0.327, Acormax=1.341, Acor_av=0.747 F test: Probability=0.000, F= 0.892 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10898, wR= 0.17305, Acormin=0.388, Acormax=1.401, Acor_av=0.838 F test: Probability=0.000, F= 0.746 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09704, wR= 0.14045, Acormin=0.254, Acormax=1.395, Acor_av=0.708 F test: Probability=0.000, F= 0.933 Trying model 5 (ne=4, no=3)... Results: Rint= 0.12476, wR= 0.16226, Acormin=0.126, Acormax=1.063, Acor_av=0.487 F test: Probability=0.000, F= 0.553 Final absorption model (ne=2, no=0): Rint= 0.09533, Acormin=0.564, Acormax=1.236, Acor_av=0.949 Combined refinement in use Rint: 0.21690 There are 36 active scales (one needs to be fixed) Refinement control: frame scale #22 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 40 pars with 820 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24962 Using Levenberg-Marquardt: 0.00010 New wR= 0.11121 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21493 with corrections 0.09093 Rint for all data: 0.21690 with corrections 0.09392 0 observations identified as outliers and rejected Cycle 2 wR= 0.11121 Using Levenberg-Marquardt: 0.00001 New wR= 0.10588 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21493 with corrections 0.08055 Rint for all data: 0.21690 with corrections 0.08361 0 observations identified as outliers and rejected Cycle 3 wR= 0.10588 Using Levenberg-Marquardt: 0.00000 New wR= 0.10467 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21493 with corrections 0.08169 Rint for all data: 0.21690 with corrections 0.08475 0 observations identified as outliers and rejected Cycle 4 wR= 0.10467 Using Levenberg-Marquardt: 0.00000 New wR= 0.10445 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21493 with corrections 0.08249 Rint for all data: 0.21690 with corrections 0.08553 0 observations identified as outliers and rejected Cycle 5 wR= 0.10445 Using Levenberg-Marquardt: 0.00000 New wR= 0.10444 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21493 with corrections 0.08330 Rint for all data: 0.21690 with corrections 0.08634 Final wR= 0.10444 Final frame scales: Min= 0.4958 Max= 1.1283 Final absorption correction factors: Amin= 0.5920 Amax= 1.2939 PROFFIT INFO: Inet (after scale3 abspack): min=-1058.9760 max=1226245.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=56.9896 max=23183.6348 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/103 1774 reflections read from tmp file 115 reflections are rejected (109 as outliers, 6 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 12 11 4 8 11 11 13 6 79 Initial Chi^2= 0.62463 Cycle 1, Chi^2= 1.05343 Current error model SIG(F2)^2 = 97.63*I_RAW + 3.05*I_BACK+(0.03831*)^2 Cycle 2, Chi^2= 1.04036 Current error model SIG(F2)^2 = 118.55*I_RAW + 0.68*I_BACK+(0.02853*)^2 Cycle 3, Chi^2= 1.00043 Current error model SIG(F2)^2 = 124.26*I_RAW + 0.70*I_BACK+(0.02812*)^2 Cycle 4, Chi^2= 0.99954 Current error model SIG(F2)^2 = 124.18*I_RAW + 0.72*I_BACK+(0.02820*)^2 Cycle 5, Chi^2= 1.00013 Current error model SIG(F2)^2 = 124.14*I_RAW + 0.72*I_BACK+(0.02819*)^2 Final Chi^2= 1.00013 Final error model SIG(F2)^2 = 124.14*I_RAW + 0.72*I_BACK+(0.02819*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1226246- 126555 177 380892.01 27.69 100.00 126407- 3678 177 28386.76 10.97 99.44 3650- 1941 177 2721.19 5.07 94.35 1939- 1149 177 1467.53 3.29 44.63 1148- 770 177 941.34 2.35 10.73 770- 505 177 653.47 2.04 7.34 505- 305 177 403.87 1.79 7.91 305- 129 177 205.84 1.32 2.82 128- 3 177 63.91 0.66 0.00 2- -1059 181 -147.63 -0.62 0.00 ------------------------------------------------------------------------------------ 1226246- -1059 1774 41464.79 5.44 36.64 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 177 101140.30 8.82 70.06 1.64- 1.26 177 75523.35 8.04 57.63 1.26- 1.09 177 59479.51 7.37 66.10 1.09- 0.97 177 50892.41 5.94 31.64 0.97- 0.88 177 18961.45 4.39 40.68 0.88- 0.81 177 45229.10 6.24 33.90 0.80- 0.76 177 17508.41 3.44 19.77 0.75- 0.71 177 22048.59 4.58 17.51 0.71- 0.67 177 21619.29 4.34 24.86 0.67- 0.63 181 3112.19 1.35 4.97 ------------------------------------------------------------------------------------ 6.00- 0.63 1774 41464.79 5.44 36.64 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 177 101140.30 8.82 70.06 6.00- 1.26 354 88331.83 8.43 63.84 6.00- 1.09 531 78714.39 8.08 64.60 6.00- 0.97 708 71758.89 7.54 56.36 6.00- 0.88 885 61199.40 6.91 53.22 6.00- 0.81 1062 58537.69 6.80 50.00 6.00- 0.76 1239 52676.36 6.32 45.68 6.00- 0.71 1416 48847.89 6.10 42.16 6.00- 0.67 1593 45822.49 5.91 40.24 6.00- 0.63 1774 41464.79 5.44 36.64 ------------------------------------------------------------------------------------ 6.00- 0.63 1774 41464.79 5.44 36.64 Scale applied to data: s=0.815496 (maximum obs:1226245.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.086; Rsigma 0.042: data 1774 -> merged 162 With outlier rejection... Rint 0.072; Rsigma 0.043: data 1756 -> merged 162 Rejected total: 18, method kkm 16, method Blessing 2 Completeness direct cell (a, b, c) = (10.420, 10.420, 10.420), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627184, 6.015739 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.76 14 14 11.29 100.00 158 1.74 - 1.27 14 14 12.64 100.00 177 1.26 - 1.06 14 14 14.29 100.00 200 1.05 - 0.97 14 14 12.21 100.00 171 0.95 - 0.88 14 14 13.14 100.00 184 0.87 - 0.81 14 14 11.50 100.00 161 0.80 - 0.76 14 14 12.07 100.00 169 0.76 - 0.72 14 14 10.29 100.00 144 0.72 - 0.69 14 14 10.71 100.00 150 0.69 - 0.65 19 19 9.37 100.00 178 --------------------------------------------------------------- 7.37 - 0.65 145 145 11.67 100.00 1692 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:41:57 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.378109 7.366083 7.386091 120.2632 120.1569 89.6364 1672 Reflections read from file xs2212a.hkl 1672 Reflections used for space-group determination (up to diffraction limit of 0.60A); mean (I/sigma) = 4.10 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 860 847 843 847 1275 1108 1106 1672 N (int>3sigma) = 0 87 83 114 74 142 220 224 332 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.8 20.7 24.1 23.0 Mean int/sigma = 0.0 1.3 1.3 1.7 1.2 1.4 3.8 4.4 4.1 Lattice type: P chosen Volume: 282.94 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.347 7.365 7.366 119.94 119.73 90.11 Niggli form: a.a = 53.975 b.b = 54.237 c.c = 54.259 b.c = -27.075 a.c = -26.840 a.b = -0.103 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.509 CUBIC F-lattice R(int) = 0.213 [ 1437] Vol = 1131.8 Cell: 10.459 10.412 10.393 89.86 90.09 89.89 Volume: 1131.75 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.422 TETRAGONAL I-lattice R(int) = 0.163 [ 1094] Vol = 565.9 Cell: 7.372 7.386 10.393 90.03 89.84 89.75 Volume: 565.88 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.330 TETRAGONAL I-lattice R(int) = 0.192 [ 1089] Vol = 565.9 Cell: 7.347 7.365 10.459 90.01 89.86 90.11 Volume: 565.88 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.263 TETRAGONAL I-lattice R(int) = 0.163 [ 1094] Vol = 565.9 Cell: 7.386 7.372 10.393 90.16 90.03 90.25 Volume: 565.88 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.351 ORTHORHOMBIC F-lattice R(int) = 0.156 [ 1074] Vol = 1131.8 Cell: 10.393 10.412 10.459 89.89 90.09 89.86 Volume: 1131.75 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.448 ORTHORHOMBIC I-lattice R(int) = 0.119 [ 1051] Vol = 565.9 Cell: 10.393 7.386 7.372 89.75 89.84 90.03 Volume: 565.88 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.185 ORTHORHOMBIC I-lattice R(int) = 0.189 [ 1051] Vol = 565.9 Cell: 7.347 7.365 10.459 89.99 90.14 90.11 Volume: 565.88 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.311 MONOCLINIC I-lattice R(int) = 0.075 [ 676] Vol = 565.9 Cell: 7.372 10.393 7.386 90.03 90.25 90.16 Volume: 565.88 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.319 MONOCLINIC I-lattice R(int) = 0.155 [ 793] Vol = 565.9 Cell: 7.366 10.412 7.378 89.98 90.36 89.82 Volume: 565.88 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.272 MONOCLINIC I-lattice R(int) = 0.075 [ 676] Vol = 565.9 Cell: 7.386 10.393 7.372 90.16 90.25 90.03 Volume: 565.88 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.112 MONOCLINIC I-lattice R(int) = 0.177 [ 750] Vol = 565.9 Cell: 7.347 7.365 10.459 90.01 90.14 89.89 Volume: 565.88 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.096 MONOCLINIC I-lattice R(int) = 0.130 [ 691] Vol = 565.9 Cell: 7.347 10.459 7.365 90.01 90.11 89.86 Volume: 565.88 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.235 MONOCLINIC I-lattice R(int) = 0.130 [ 691] Vol = 565.9 Cell: 7.347 10.459 7.365 89.99 90.11 90.14 Volume: 565.88 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.067 [ 309] Vol = 282.9 Cell: 7.347 7.365 7.366 119.94 119.73 90.11 Volume: 282.94 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 0 843 0 1110 1113 1672 N (int>3sigma) = 0 0 0 0 114 0 233 232 332 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 24.6 22.6 23.0 Mean int/sigma = 0.0 0.0 0.0 0.0 1.7 0.0 4.2 4.1 4.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.982 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 10 10 133 302 N I>3s 0 0 0 68 0.1 0.1 -0.0 1.4 0.7 0.7 0.1 2.2 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 0.213 1332 Fd-3m 1 1 227 C N N N N 37 2284 0.214 1394 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.458750 10.412385 10.392588 89.8610 90.0935 89.8911 ZERR 1.00 0.001429 0.015359 0.008170 0.0006 0.0018 0.1644 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1087340- 91312 213 200 27 7.4 327926.54 25.83 0.067 0.070 77738- 1657 335 332 27 12.3 5139.22 6.84 0.124 0.143 1574- 739 329 328 27 12.1 1145.68 2.63 0.245 0.300 732- 355 335 335 27 12.4 534.16 1.85 0.392 0.482 347- 71 293 292 27 10.8 221.66 1.12 0.593 0.890 64- -343 269 269 27 10.0 -5.30 0.12 0.968 3.407 ------------------------------------------------------------------------------------------- 1087340- -343 1774 1756 162 10.8 38672.87 5.28 0.072 0.074 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-1.27 338 333 27 12.3 84942.83 8.46 0.069 0.066 0.032 1.26-0.97 358 354 27 13.1 50717.62 6.35 0.058 0.065 0.038 0.97-0.81 338 334 27 12.4 31978.03 5.38 0.079 0.083 0.049 0.81-0.73 318 316 27 11.7 10301.87 2.68 0.089 0.093 0.075 0.73-0.67 258 256 27 9.5 28194.35 5.25 0.091 0.102 0.062 0.67-0.63 164 163 27 6.0 3164.10 1.38 0.271 0.210 0.162 ------------------------------------------------------------------------------------------------------ inf-0.63 1774 1756 162 10.8 38672.87 5.28 0.072 0.074 0.043 inf-0.65 1707 1690 144 11.7 39970.62 5.43 0.071 0.073 0.042 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-1.27 333 27 27 100.0 12.3 84942.83 29.11 0.069 0.015 1.26-0.97 354 27 27 100.0 13.1 50717.62 22.46 0.058 0.014 0.97-0.81 334 27 27 100.0 12.4 31978.03 19.21 0.079 0.018 0.81-0.73 316 27 27 100.0 11.7 10301.87 8.55 0.089 0.026 0.73-0.67 256 27 27 100.0 9.5 28194.35 16.81 0.091 0.021 0.67-0.63 163 27 27 100.0 6.0 3164.10 3.52 0.271 0.079 -------------------------------------------------------------------------------------------- inf-0.63 1756 162 162 100.0 10.8 38672.87 18.02 0.072 0.017 inf-0.65 1690 144 144 100.0 11.7 39970.62 18.62 0.071 0.016 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:48:44 2019) ID: 3668; threads 40; handles 811; mem 515516.00 (1204688.00)kB; time: 1w 4d 22h 59m 32s MEMORY INFO: Memory PF:280.0, Ph:669.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.4,peak PF: 700.2, WS: 471.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:282.0, Ph:671.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.2,peak PF: 700.2, WS: 473.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:48:44 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000103 0.000065 0.000100 ) 0.064809 0.092374 0.027273 ( 0.000110 0.000070 0.000107 ) 0.045523 0.057900 0.132205 ( 0.000124 0.000079 0.000121 ) 7.38096 ( 0.00728 ) 7.36649 ( 0.00751 ) 7.42630 ( 0.00809 ) 120.52449 ( 0.11168 ) 120.40327 ( 0.10963 ) 89.27095 ( 0.08125 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:48:44 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000103 0.000065 0.000100 ) 0.064809 0.092374 0.027273 ( 0.000110 0.000070 0.000107 ) 0.045523 0.057900 0.132205 ( 0.000124 0.000079 0.000121 ) M - matrix: 0.013831 0.004557 0.009207 ( 0.000025 0.000016 0.000021 ) 0.004557 0.013965 0.009324 ( 0.000016 0.000017 0.000017 ) 0.009207 0.009324 0.018445 ( 0.000021 0.000017 0.000033 ) unit cell: 7.381(7) 7.366(7) 7.426(8) 120.52(11) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** 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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb PROFFITPEAK info: 501 peaks in the peak location table UB fit with 60 obs out of 270 (total:270,skipped:0) (22.22%) UB - matrix: 0.086639 -0.046672 0.015876 ( 0.000601 0.000364 0.000706 ) 0.063049 0.092085 0.026344 ( 0.000568 0.000344 0.000668 ) 0.046370 0.058421 0.133647 ( 0.000887 0.000537 0.001043 ) M - matrix: 0.013632 0.004471 0.009234 ( 0.000151 0.000091 0.000149 ) 0.004471 0.014071 0.009493 ( 0.000091 0.000095 0.000118 ) 0.009234 0.009493 0.018807 ( 0.000149 0.000118 0.000282 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.3(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 270 #indexed refl 253, indexation with best UB: 93.7037% Lattice: 7.3815 7.3768 7.3518 120.333 120.100 89.497 282.447 Rotation: -23.970 24.246 -35.217 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 255 obs out of 270 (total:270,skipped:0) (94.44%) UB - matrix: 0.087628 -0.045091 0.014237 ( 0.000066 0.000079 0.000085 ) 0.061847 0.092765 0.025204 ( 0.000074 0.000088 0.000095 ) 0.048295 0.057125 0.133605 ( 0.000055 0.000066 0.000071 ) M - matrix: 0.013836 0.004545 0.009259 ( 0.000016 0.000012 0.000013 ) 0.004545 0.013902 0.009328 ( 0.000012 0.000019 0.000014 ) 0.009259 0.009328 0.018688 ( 0.000013 0.000014 0.000020 ) unit cell: 7.376(6) 7.377(7) 7.352(5) 120.33(9) 120.08(8) 89.52(7) V = 282.3(4) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB - matrix: 0.087590 -0.045001 0.014151 ( 0.000061 0.000073 0.000079 ) 0.061858 0.092877 0.025084 ( 0.000073 0.000087 0.000095 ) 0.048492 0.057084 0.133659 ( 0.000060 0.000072 0.000078 ) M - matrix: 0.013850 0.004572 0.009273 ( 0.000015 0.000012 0.000013 ) 0.004572 0.013910 0.009323 ( 0.000012 0.000019 0.000014 ) 0.009273 0.009323 0.018694 ( 0.000013 0.000014 0.000021 ) UB fit with 254 obs out of 270 (total:270,skipped:0) (94.07%) unit cell: 7.375(6) 7.371(7) 7.346(6) 120.21(9) 120.05(8) 89.68(7) V = 282.0(4) UB fit with 254 obs out of 270 (total:270,skipped:0) (94.07%) UB - matrix: 0.087590 -0.045001 0.014151 ( 0.000061 0.000073 0.000079 ) 0.061858 0.092877 0.025084 ( 0.000073 0.000087 0.000095 ) 0.048492 0.057084 0.133659 ( 0.000060 0.000072 0.000078 ) M - matrix: 0.013850 0.004572 0.009273 ( 0.000015 0.000012 0.000013 ) 0.004572 0.013910 0.009323 ( 0.000012 0.000019 0.000014 ) 0.009273 0.009323 0.018694 ( 0.000013 0.000014 0.000021 ) unit cell: 7.375(6) 7.371(7) 7.346(6) 120.21(9) 120.05(8) 89.68(7) V = 282.0(4) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB - matrix: 0.087590 -0.045001 0.014151 ( 0.000061 0.000073 0.000079 ) 0.061858 0.092877 0.025084 ( 0.000073 0.000087 0.000095 ) 0.048492 0.057084 0.133659 ( 0.000060 0.000072 0.000078 ) M - matrix: 0.013850 0.004572 0.009273 ( 0.000015 0.000012 0.000013 ) 0.004572 0.013910 0.009323 ( 0.000012 0.000019 0.000014 ) 0.009273 0.009323 0.018694 ( 0.000013 0.000014 0.000021 ) UB fit with 254 obs out of 270 (total:270,skipped:0) (94.07%) unit cell: 7.375(6) 7.371(7) 7.346(6) 120.21(9) 120.05(8) 89.68(7) V = 282.0(4) 270 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Run 2 Omega scan: (-49.000 - 51.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1270 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087590 -0.045001 0.014151 ( 0.000061 0.000073 0.000079 ) 0.061858 0.092877 0.025084 ( 0.000073 0.000087 0.000095 ) 0.048492 0.057084 0.133659 ( 0.000060 0.000072 0.000078 ) M - matrix: 0.013850 0.004572 0.009273 ( 0.000015 0.000012 0.000013 ) 0.004572 0.013910 0.009323 ( 0.000012 0.000019 0.000014 ) 0.009273 0.009323 0.018694 ( 0.000013 0.000014 0.000021 ) UB fit with 254 obs out of 270 (total:270,skipped:0) (94.07%) unit cell: 7.375(6) 7.371(7) 7.346(6) 120.21(9) 120.05(8) 89.68(7) V = 282.0(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 255 obs out of 270 (total:270,skipped:0) (94.44%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb 0 of 247 peaks identified as outliers and rejected 247 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 247 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 247 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.001 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.103) | 0.883 ( 0.155) | 1.062 ( 0.554) | 1.75- 1.58 | 25 | 0.910 ( 0.079) | 0.903 ( 0.137) | 0.957 ( 0.357) | 1.57- 1.35 | 25 | 0.929 ( 0.082) | 0.955 ( 0.111) | 0.867 ( 0.383) | 1.35- 1.19 | 25 | 0.935 ( 0.075) | 0.942 ( 0.109) | 1.051 ( 0.618) | 1.16- 1.06 | 25 | 0.910 ( 0.066) | 0.948 ( 0.119) | 0.782 ( 0.321) | 1.06- 0.89 | 25 | 0.960 ( 0.056) | 0.983 ( 0.112) | 1.057 ( 0.418) | 0.89- 0.82 | 25 | 0.936 ( 0.070) | 0.923 ( 0.084) | 1.158 ( 0.393) | 0.82- 0.69 | 25 | 0.955 ( 0.051) | 0.916 ( 0.101) | 1.343 ( 0.480) | 0.69- 0.63 | 22 | 0.929 ( 0.036) | 0.870 ( 0.075) | 1.394 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 0.63 | 247 | 0.920 ( 0.080) | 0.920 ( 0.121) | 1.063 ( 0.488) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 247 obs out of 247 (total:247,skipped:0) (100.00%) UB - matrix: 0.087527 -0.045134 0.014097 ( 0.000042 0.000052 0.000056 ) 0.061983 0.093193 0.025286 ( 0.000038 0.000046 0.000050 ) 0.048736 0.057091 0.133872 ( 0.000041 0.000051 0.000055 ) M - matrix: 0.013878 0.004608 0.009326 ( 0.000010 0.000008 0.000008 ) 0.004608 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009326 0.009363 0.018760 ( 0.000008 0.000009 0.000015 ) unit cell: 7.378(4) 7.352(4) 7.340(4) 120.16(5) 120.15(5) 89.71(4) V = 280.9(2) OTKP changes: 247 1 1 1 OTKP changes: 247 1 1 1 OTKP changes: 247 1 1 1 UB - matrix: 0.087520 -0.045144 0.014079 ( 0.000045 0.000055 0.000059 ) 0.062002 0.092994 0.025363 ( 0.000037 0.000045 0.000049 ) 0.048472 0.057073 0.133678 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013854 0.004581 0.009284 ( 0.000010 0.000007 0.000007 ) 0.004581 0.013943 0.009352 ( 0.000007 0.000011 0.000008 ) 0.009284 0.009352 0.018711 ( 0.000007 0.000008 0.000011 ) UB fit with 247 obs out of 247 (total:247,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.28(5) 120.08(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 51.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087520 -0.045144 0.014079 ( 0.000045 0.000055 0.000059 ) 0.062002 0.092994 0.025363 ( 0.000037 0.000045 0.000049 ) 0.048472 0.057073 0.133678 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013854 0.004581 0.009284 ( 0.000010 0.000007 0.000007 ) 0.004581 0.013943 0.009352 ( 0.000007 0.000011 0.000008 ) 0.009284 0.009352 0.018711 ( 0.000007 0.000008 0.000011 ) UB fit with 247 obs out of 247 (total:247,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.28(5) 120.08(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 247 obs out of 247 (total:247,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb 0 of 250 peaks identified as outliers and rejected 250 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 250 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 250 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.870 ( 0.090) | 0.870 ( 0.127) | 1.027 ( 0.496) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.976 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.899 ( 0.155) | 0.997 ( 0.427) | 1.58- 1.35 | 25 | 0.952 ( 0.070) | 0.967 ( 0.107) | 0.875 ( 0.443) | 1.35- 1.19 | 25 | 0.920 ( 0.067) | 0.919 ( 0.118) | 1.018 ( 0.602) | 1.19- 1.06 | 25 | 0.926 ( 0.069) | 0.968 ( 0.104) | 0.819 ( 0.285) | 1.06- 0.91 | 25 | 0.964 ( 0.064) | 0.982 ( 0.094) | 1.126 ( 0.457) | 0.89- 0.82 | 25 | 0.942 ( 0.068) | 0.936 ( 0.094) | 1.057 ( 0.404) | 0.82- 0.72 | 25 | 0.948 ( 0.050) | 0.911 ( 0.098) | 1.315 ( 0.425) | 0.72- 0.63 | 25 | 0.931 ( 0.035) | 0.877 ( 0.089) | 1.379 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 250 | 0.923 ( 0.079) | 0.922 ( 0.121) | 1.059 ( 0.489) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-11.3 | 46 | 0.973 ( 0.039) | 1.010 ( 0.084) | 1.156 ( 0.467) | 11.3-15.1 | 46 | 0.980 ( 0.044) | 1.045 ( 0.071) | 1.181 ( 0.540) | 15.2-19.6 | 46 | 1.000 ( 0.305) | 1.018 ( 0.112) | 1.287 ( 1.534) | 19.7-23.9 | 46 | 0.951 ( 0.050) | 0.999 ( 0.078) | 0.935 ( 0.410) | 24.0-27.3 | 46 | 0.946 ( 0.068) | 0.990 ( 0.103) | 0.964 ( 0.454) | 27.4-32.6 | 46 | 0.937 ( 0.100) | 0.948 ( 0.121) | 0.977 ( 0.471) | 32.7-36.3 | 46 | 0.920 ( 0.211) | 0.888 ( 0.121) | 1.122 ( 0.780) | 36.4-38.9 | 46 | 0.861 ( 0.085) | 0.828 ( 0.117) | 1.008 ( 0.514) | 39.0-41.6 | 46 | 0.882 ( 0.088) | 0.832 ( 0.129) | 1.084 ( 0.452) | 41.7-50.1 | 48 | 0.867 ( 0.105) | 0.786 ( 0.119) | 1.081 ( 0.553) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 462 | 0.931 ( 0.143) | 0.934 ( 0.139) | 1.079 ( 0.703) | Fitted profile normalization line parameters e1 dimension: a=-0.0036 b=1.14 e2 dimension: a=-0.0078 b=1.27 e3 dimension: a=0.0051 b=0.93 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5513 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386424 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336515 PROFFITPEAK - Finished at Wed Aug 21 12:48:52 2019 PROFFITMAIN - Started at Wed Aug 21 12:48:52 2019 OTKP changes: 255 2 1 2 OTKP changes: 255 2 1 2 OTKP changes: 255 2 1 2 UB - matrix: 0.087547 -0.046033 0.017099 ( 0.000097 0.000061 0.000095 ) 0.064106 0.092432 0.027172 ( 0.000104 0.000066 0.000102 ) 0.045416 0.057710 0.132116 ( 0.000110 0.000070 0.000108 ) M - matrix: 0.013837 0.004516 0.009239 ( 0.000024 0.000014 0.000019 ) 0.004516 0.013993 0.009349 ( 0.000014 0.000016 0.000015 ) 0.009239 0.009349 0.018485 ( 0.000019 0.000015 0.000029 ) UB fit with 275 obs out of 462 (total:462,skipped:0) (59.52%) unit cell: 7.388(7) 7.370(7) 7.430(7) 120.67(10) 120.36(10) 89.03(8) V = 284.0(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 202 obs out of 212 (total:212,skipped:0) (95.28%) UB - matrix: 0.087481 -0.046132 0.017384 ( 0.000099 0.000061 0.000092 ) 0.064755 0.092358 0.027243 ( 0.000086 0.000054 0.000080 ) 0.045705 0.057840 0.132147 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013935 0.004589 0.009325 ( 0.000023 0.000013 0.000018 ) 0.004589 0.014004 0.009358 ( 0.000013 0.000014 0.000013 ) 0.009325 0.009358 0.018507 ( 0.000018 0.000013 0.000026 ) unit cell: 7.381(6) 7.367(6) 7.434(6) 120.52(9) 120.47(9) 89.22(7) V = 283.5(4) OTKP changes: 200 1 1 1 OTKP changes: 200 1 1 1 OTKP changes: 200 1 1 1 UB - matrix: 0.087357 -0.045952 0.017474 ( 0.000098 0.000061 0.000092 ) 0.064664 0.092297 0.027268 ( 0.000086 0.000053 0.000081 ) 0.045527 0.057801 0.132003 ( 0.000102 0.000063 0.000096 ) M - matrix: 0.013885 0.004586 0.009299 ( 0.000022 0.000013 0.000017 ) 0.004586 0.013971 0.009344 ( 0.000013 0.000013 0.000013 ) 0.009299 0.009344 0.018474 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.394(6) 7.377(6) 7.441(6) 120.52(9) 120.44(9) 89.27(7) V = 284.6(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.107) HKL list info: 1300 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087357 -0.045952 0.017474 ( 0.000098 0.000061 0.000092 ) 0.064664 0.092297 0.027268 ( 0.000086 0.000053 0.000081 ) 0.045526 0.057801 0.132003 ( 0.000102 0.000064 0.000096 ) M - matrix: 0.013885 0.004585 0.009299 ( 0.000022 0.000013 0.000017 ) 0.004585 0.013971 0.009344 ( 0.000013 0.000013 0.000013 ) 0.009299 0.009344 0.018474 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.394(6) 7.377(6) 7.441(6) 120.52(9) 120.44(9) 89.27(7) V = 284.6(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118029 0.039095 0.078775 ( 0.000075 0.000047 0.000069 ) 0.000036 0.111506 0.056219 ( 0.000075 0.000047 0.000070 ) 0.000027 -0.000046 0.095481 ( 0.000090 0.000056 0.000084 ) M - matrix: 0.013931 0.004618 0.009302 ( 0.000018 0.000010 0.000014 ) 0.004618 0.013962 0.009344 ( 0.000010 0.000011 0.000011 ) 0.009302 0.009344 0.018483 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.376(5) 7.380(5) 7.428(8) 120.46(9) 120.29(9) 89.48(5) V = 284.0(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 250 obs out of 250 (total:250,skipped:0) (100.00%) UB - matrix: 0.087515 -0.045144 0.014074 ( 0.000045 0.000055 0.000059 ) 0.062033 0.093013 0.025369 ( 0.000037 0.000046 0.000049 ) 0.048476 0.057088 0.133714 ( 0.000029 0.000036 0.000039 ) M - matrix: 0.013857 0.004586 0.009287 ( 0.000009 0.000007 0.000007 ) 0.004586 0.013948 0.009358 ( 0.000007 0.000011 0.000008 ) 0.009287 0.009358 0.018721 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.367(4) 7.347(3) 120.28(5) 120.07(5) 89.65(4) V = 281.6(2) OTKP changes: 250 1 1 1 OTKP changes: 250 1 1 1 OTKP changes: 250 1 1 1 UB - matrix: 0.087501 -0.045140 0.014059 ( 0.000045 0.000055 0.000059 ) 0.062031 0.092987 0.025363 ( 0.000037 0.000046 0.000049 ) 0.048454 0.057076 0.133690 ( 0.000029 0.000035 0.000038 ) M - matrix: 0.013852 0.004584 0.009281 ( 0.000009 0.000007 0.000007 ) 0.004584 0.013942 0.009354 ( 0.000007 0.000011 0.000008 ) 0.009281 0.009354 0.018714 ( 0.000007 0.000008 0.000011 ) UB fit with 250 obs out of 250 (total:250,skipped:0) (100.00%) unit cell: 7.376(4) 7.369(4) 7.348(3) 120.28(5) 120.05(5) 89.66(4) V = 281.8(2) Run 2 Omega scan: (-49.000 - 51.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1262 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087501 -0.045140 0.014059 ( 0.000045 0.000055 0.000059 ) 0.062031 0.092987 0.025363 ( 0.000037 0.000046 0.000049 ) 0.048454 0.057076 0.133690 ( 0.000029 0.000035 0.000038 ) M - matrix: 0.013852 0.004584 0.009281 ( 0.000009 0.000007 0.000007 ) 0.004584 0.013942 0.009354 ( 0.000007 0.000011 0.000008 ) 0.009281 0.009354 0.018714 ( 0.000007 0.000008 0.000011 ) UB fit with 250 obs out of 250 (total:250,skipped:0) (100.00%) unit cell: 7.376(4) 7.369(4) 7.348(3) 120.28(5) 120.05(5) 89.66(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 250 obs out of 250 (total:250,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117847 0.039183 0.078924 ( 0.000031 0.000039 0.000041 ) 0.000016 0.111460 0.056247 ( 0.000035 0.000043 0.000046 ) -0.000034 -0.000019 0.096459 ( 0.000027 0.000033 0.000035 ) M - matrix: 0.013888 0.004619 0.009299 ( 0.000007 0.000006 0.000006 ) 0.004619 0.013959 0.009360 ( 0.000006 0.000010 0.000007 ) 0.009299 0.009360 0.018697 ( 0.000006 0.000007 0.000011 ) UB fit with 250 obs out of 250 (total:250,skipped:0) (100.00%) unit cell: 7.370(2) 7.366(3) 7.351(3) 120.23(5) 120.03(4) 89.78(3) V = 281.59(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 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\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_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\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117847 0.039062 0.078705 ( 0.000040 0.000035 0.000042 ) -0.000014 0.111485 0.056241 ( 0.000038 0.000033 0.000040 ) -0.000007 -0.000152 0.095994 ( 0.000048 0.000042 0.000050 ) M - matrix: 0.013888 0.004602 0.009274 ( 0.000009 0.000006 0.000008 ) 0.004602 0.013955 0.009330 ( 0.000006 0.000008 0.000007 ) 0.009274 0.009330 0.018572 ( 0.000008 0.000007 0.000012 ) UB fit with 457 obs out of 462 (total:462,skipped:0) (98.92%) unit cell: 7.372(3) 7.368(3) 7.383(5) 120.29(5) 120.11(5) 89.65(3) V = 282.7(2) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 62 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof 2031 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:48:55 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.107) Run 2 Omega scan: (-49.000 - 51.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-552.0000 max=7876303.0000 PROFFIT INFO: signal sum lp corr: min=-608.8097 max=1117577.7511 PROFFIT INFO: background sum: min=130.0000 max=7706.0000 PROFFIT INFO: background sum sig2: min=387.0000 max=5044.0000 PROFFIT INFO: num of signal pixels: min=39 max=502 PROFFIT INFO: Inet: min=-974.0956 max=1788124.3750 PROFFIT INFO: sig(Inet): min=64.6188 max=24252.3379 PROFFIT INFO: Inet/sig(Inet): min=-1.59 max=180.79 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 186 714 1054 1269 1364 1581 1713 1789 1923 2012 2031 Percent 9.2 35.2 51.9 62.5 67.2 77.8 84.3 88.1 94.7 99.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2031 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 2031 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1788124- 132318 203 397751.49 75.62 100.00 132268- 4086 203 30356.94 20.03 100.00 4070- 2114 203 2890.18 7.18 98.03 2113- 1255 203 1624.06 3.93 51.23 1253- 824 203 1029.42 2.18 11.82 819- 552 203 676.86 1.63 5.91 549- 324 203 431.48 1.30 7.88 323- 146 203 227.41 0.66 0.49 145- 9 203 75.28 0.27 0.00 8- -974 204 -143.36 -0.27 0.00 ------------------------------------------------------------------------------------ 1788124- -974 2031 43470.49 11.25 37.52 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 203 94739.46 15.68 68.47 1.75- 1.26 203 91682.87 21.29 58.62 1.26- 1.06 203 49617.26 13.62 49.75 1.06- 0.93 203 35819.28 11.52 43.35 0.93- 0.84 203 43515.00 12.67 33.00 0.84- 0.76 203 30456.86 9.68 33.00 0.76- 0.71 203 31576.75 9.26 30.54 0.71- 0.65 203 17455.98 5.89 18.23 0.65- 0.59 203 24402.66 7.67 24.14 0.59- 0.46 204 15576.23 5.19 16.18 ------------------------------------------------------------------------------------ 6.55- 0.46 2031 43470.49 11.25 37.52 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:48:55 2019 Sorting 2031 observations 71 unique observations with > 7.00 F2/sig(F2) 2031 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 98 202 Total number of frames 202 Maximum number of 71 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 2031 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 32 68 Total number of frames 68 489 observations > 7.00 F2/sig(F2) 489 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 32 68 Total number of frames 68 Removing 'redundancy=1' reflections Average redundancy: 4.6 (Out of 489 removed 40 = 449, unique = 97) 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 449 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 32 68 Total number of frames 68 97 unique data precomputed (should be 97) 97 unique data with 449 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.6 (Out of 449 removed 0 = 449, unique = 97) 97 unique data precomputed (should be 97) 97 unique data with 449 observations RMS deviation of equivalent data = 0.37684 Rint = 0.35445 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.35445, wR= 0.47433 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26925, wR= 0.36075, Acormin=0.338, Acormax=1.453, Acor_av=0.828 F test: Probability=1.000, F= 1.708 Trying model 2 (ne=2, no=1)... Results: Rint= 0.31231, wR= 0.38164, Acormin=0.061, Acormax=1.629, Acor_av=0.593 F test: Probability=0.000, F= 0.737 Trying model 3 (ne=4, no=0)... Results: Rint= 0.29145, wR= 0.32940, Acormin=0.057, Acormax=1.873, Acor_av=0.696 F test: Probability=0.000, F= 0.831 Trying model 4 (ne=4, no=1)... Results: Rint= 0.33099, wR= 0.34618, Acormin=-0.014, Acormax=1.650, Acor_av=0.500 F test: Probability=0.000, F= 0.639 Trying model 5 (ne=4, no=3)... Results: Rint= 0.37266, wR= 0.37420, Acormin=-0.113, Acormax=2.031, Acor_av=0.307 F test: Probability=0.000, F= 0.493 Trying model 6 (ne=6, no=0)... Results: Rint= 0.29405, wR= 0.34360, Acormin=-0.103, Acormax=1.857, Acor_av=0.552 F test: Probability=0.000, F= 0.785 Trying model 7 (ne=6, no=1)... Results: Rint= 0.33467, wR= 0.35358, Acormin=0.023, Acormax=1.545, Acor_av=0.449 F test: Probability=0.000, F= 0.601 Trying model 8 (ne=6, no=3)... Results: Rint= 0.32251, wR= 0.33609, Acormin=-0.125, Acormax=2.056, Acor_av=0.328 F test: Probability=0.000, F= 0.633 Trying model 9 (ne=6, no=5)... Results: Rint= 0.30108, wR= 0.37074, Acormin=-0.120, Acormax=2.759, Acor_av=0.133 F test: Probability=0.000, F= 0.701 Trying model 10 (ne=8, no=0)... Results: Rint= 0.31943, wR= 0.38711, Acormin=-0.126, Acormax=1.871, Acor_av=0.385 F test: Probability=0.000, F= 0.631 Trying model 11 (ne=8, no=1)... Results: Rint= 0.42610, wR= 0.45475, Acormin=-0.112, Acormax=1.411, Acor_av=0.242 F test: Probability=0.000, F= 0.351 Trying model 12 (ne=8, no=3)... Results: Rint= 0.20495, wR= 0.23406, Acormin=-0.017, Acormax=0.187, Acor_av=0.058 F test: Probability=1.000, F= 1.482 Trying model 13 (ne=8, no=5)... Results: Rint= 0.18590, wR= 0.20638, Acormin=-0.019, Acormax=0.191, Acor_av=0.065 F test: Probability=1.000, F= 1.735 Trying model 14 (ne=8, no=7)... Results: Rint= 0.13113, wR= 0.17392, Acormin=0.010, Acormax=0.263, Acor_av=0.078 F test: Probability=1.000, F= 3.305 Final absorption model (ne=2, no=0): Rint= 0.26925, Acormin=0.338, Acormax=1.453, Acor_av=0.828 Combined refinement in use Rint: 0.36930 There are 68 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 72 pars with 2628 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.37684 Using Levenberg-Marquardt: 0.00010 New wR= 0.20056 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35445 with corrections 0.16746 Rint for all data: 0.36930 with corrections 0.18459 0 observations identified as outliers and rejected Cycle 2 wR= 0.20056 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= 0.33174 Using Levenberg-Marquardt: 0.10000 New wR= 0.19012 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35445 with corrections 0.16362 Rint for all data: 0.36930 with corrections 0.18080 0 observations identified as outliers and rejected Cycle 3 wR= 0.19012 Using Levenberg-Marquardt: 0.01000 New wR= 0.18760 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35445 with corrections 0.16457 Rint for all data: 0.36930 with corrections 0.18172 0 observations identified as outliers and rejected Cycle 4 wR= 0.18760 Using Levenberg-Marquardt: 0.00100 New wR= 0.18678 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35445 with corrections 0.16497 Rint for all data: 0.36930 with corrections 0.18210 0 observations identified as outliers and rejected Cycle 5 wR= 0.18678 Using Levenberg-Marquardt: 0.00010 New wR= 0.18624 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35445 with corrections 0.16490 Rint for all data: 0.36930 with corrections 0.18203 0 observations identified as outliers and rejected Final wR= 0.18624 Final frame scales: Min= 0.4665 Max= 1.8386 Final absorption correction factors: Amin= 0.4455 Amax= 1.3648 PROFFIT INFO: Inet (after scale3 abspack): min=-1477.1062 max=1408639.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=42.3430 max=25658.5957 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/103 2031 reflections read from tmp file 565 reflections are rejected (488 as outliers, 77 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 65 64 41 31 35 27 20 12 14 Initial Chi^2= 2.55941 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.71111 Current error model SIG(F2)^2 = 571.09*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 406.11*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 406.11*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1408639- 125922 203 358570.47 32.27 100.00 124386- 4043 203 27168.24 7.00 85.71 4034- 1941 203 2707.44 2.75 27.59 1941- 1163 203 1535.18 1.96 15.76 1163- 738 203 942.31 1.47 3.94 738- 479 203 614.04 1.11 0.49 478- 284 203 377.03 1.05 0.49 284- 133 203 209.16 0.88 1.48 133- 7 203 69.15 0.46 0.00 7- -1477 204 -171.95 -0.35 0.00 ------------------------------------------------------------------------------------ 1408639- -1477 2031 39182.72 4.86 23.54 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 203 88502.61 10.61 52.22 1.75- 1.26 203 87921.90 9.16 41.38 1.26- 1.06 203 43761.43 5.94 30.54 1.06- 0.93 203 40878.63 4.20 20.20 0.93- 0.84 203 34944.85 4.52 19.21 0.84- 0.76 203 29281.75 3.56 16.75 0.76- 0.71 203 25264.05 3.39 17.73 0.71- 0.65 203 12766.60 2.32 8.87 0.65- 0.59 203 19137.42 2.89 17.24 0.59- 0.46 204 9514.13 2.02 11.27 ------------------------------------------------------------------------------------ 6.55- 0.46 2031 39182.72 4.86 23.54 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 203 88502.61 10.61 52.22 6.55- 1.26 406 88212.26 9.88 46.80 6.55- 1.06 609 73395.31 8.57 41.38 6.55- 0.93 812 65266.14 7.48 36.08 6.55- 0.84 1015 59201.89 6.88 32.71 6.55- 0.76 1218 54215.20 6.33 30.05 6.55- 0.71 1421 50079.32 5.91 28.29 6.55- 0.65 1624 45415.23 5.46 25.86 6.55- 0.59 1827 42495.47 5.17 24.90 6.55- 0.46 2031 39182.72 4.86 23.54 ------------------------------------------------------------------------------------ 6.55- 0.46 2031 39182.72 4.86 23.54 Scale applied to data: s=0.709904 (maximum obs:1408639.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.182; Rsigma 0.051: data 2031 -> merged 390 With outlier rejection... Rint 0.151; Rsigma 0.052: data 1941 -> merged 390 Rejected total: 90, method kkm 86, method Blessing 4 Completeness direct cell (a, b, c) = (6.563, 6.563, 6.563), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.457273, 6.563105 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.59 22 22 10.23 100.00 225 1.55 - 1.22 22 22 9.73 100.00 214 1.20 - 1.02 22 22 8.91 100.00 196 1.02 - 0.92 22 22 7.45 100.00 164 0.92 - 0.84 22 22 7.36 100.00 162 0.84 - 0.79 22 22 6.00 100.00 132 0.79 - 0.75 22 22 6.00 100.00 132 0.75 - 0.71 22 22 4.64 100.00 102 0.71 - 0.69 22 22 4.91 100.00 108 0.68 - 0.65 26 29 4.58 89.66 119 --------------------------------------------------------------- 7.37 - 0.65 224 227 6.94 98.68 1554 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:48:56 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.372177 7.367920 7.382795 120.2911 120.1112 89.6484 1941 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 990 974 974 979 1469 1292 1296 1941 N (int>3sigma) = 0 110 109 151 107 185 286 291 424 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 24.0 27.3 25.5 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.2 4.9 4.6 Lattice type: P chosen Volume: 282.70 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.343 7.365 7.368 119.96 119.75 90.10 Niggli form: a.a = 53.918 b.b = 54.245 c.c = 54.286 b.c = -27.104 a.c = -26.849 a.b = -0.097 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.419 CUBIC F-lattice R(int) = 0.211 [ 1705] Vol = 1130.8 Cell: 10.455 10.409 10.391 89.83 90.03 89.90 Volume: 1130.80 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.532 TETRAGONAL I-lattice R(int) = 0.157 [ 1356] Vol = 565.4 Cell: 7.370 7.383 10.391 90.10 89.85 89.75 Volume: 565.40 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.386 TETRAGONAL I-lattice R(int) = 0.200 [ 1353] Vol = 565.4 Cell: 7.343 7.365 10.455 90.04 89.91 90.10 Volume: 565.40 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.206 TETRAGONAL I-lattice R(int) = 0.157 [ 1356] Vol = 565.4 Cell: 7.383 7.370 10.391 90.15 90.10 90.25 Volume: 565.40 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.439 ORTHORHOMBIC F-lattice R(int) = 0.165 [ 1331] Vol = 1130.8 Cell: 10.391 10.409 10.455 89.90 90.03 89.83 Volume: 1130.80 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.546 ORTHORHOMBIC I-lattice R(int) = 0.128 [ 1305] Vol = 565.4 Cell: 10.391 7.383 7.370 89.75 89.85 90.10 Volume: 565.40 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.148 ORTHORHOMBIC I-lattice R(int) = 0.201 [ 1312] Vol = 565.4 Cell: 7.343 7.365 10.455 89.96 90.09 90.10 Volume: 565.40 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.355 MONOCLINIC I-lattice R(int) = 0.094 [ 911] Vol = 565.4 Cell: 7.370 10.391 7.383 90.10 90.25 90.15 Volume: 565.40 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.378 MONOCLINIC I-lattice R(int) = 0.160 [ 995] Vol = 565.4 Cell: 7.368 10.409 7.372 89.95 90.35 89.81 Volume: 565.40 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.340 MONOCLINIC I-lattice R(int) = 0.094 [ 911] Vol = 565.4 Cell: 7.383 10.391 7.370 90.15 90.25 90.10 Volume: 565.40 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.099 MONOCLINIC I-lattice R(int) = 0.189 [ 994] Vol = 565.4 Cell: 7.343 7.365 10.455 90.04 90.09 89.90 Volume: 565.40 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.068 MONOCLINIC I-lattice R(int) = 0.155 [ 896] Vol = 565.4 Cell: 7.343 10.455 7.365 90.04 90.10 89.91 Volume: 565.40 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.125 MONOCLINIC I-lattice R(int) = 0.155 [ 896] Vol = 565.4 Cell: 7.343 10.455 7.365 89.96 90.10 90.09 Volume: 565.40 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.082 [ 371] Vol = 282.7 Cell: 7.343 7.365 7.368 119.96 119.75 90.10 Volume: 282.70 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 0 974 0 1285 1299 1941 N (int>3sigma) = 0 0 0 0 151 0 293 296 424 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 26.8 25.3 25.5 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.6 4.6 4.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.770 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 12 12 147 360 N I>3s 0 0 0 91 0.1 0.1 -0.0 1.7 0.8 0.8 0.1 2.6 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 0.211 1586 Fd-3m 1 1 227 C N N N N 37 2284 0.213 1649 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.454754 10.409449 10.390794 89.8271 90.0331 89.9041 ZERR 1.00 0.001250 0.013299 0.007175 0.0000 0.0006 0.1373 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 902015- 116513 217 191 39 4.9 340353.52 30.94 0.133 0.121 109081- 2760 224 214 39 5.5 15196.62 4.86 0.271 0.161 2747- 1516 344 327 39 8.4 1953.73 2.17 0.825 0.924 1513- 1086 274 264 39 6.8 1154.96 1.43 0.738 0.784 1080- 821 213 209 39 5.4 893.16 1.25 0.629 0.666 819- 618 175 168 39 4.3 617.96 0.99 0.687 0.725 616- 458 194 185 39 4.7 478.18 0.83 0.733 0.859 458- 347 160 158 39 4.1 389.94 0.75 0.662 0.843 344- 143 126 123 39 3.2 233.48 0.60 0.742 0.870 137- -1021 104 102 39 2.6 39.73 0.24 0.906 2.470 ------------------------------------------------------------------------------------------- 902015- -1021 2031 1941 390 5.0 35897.33 4.55 0.151 0.135 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-1.26 421 402 40 10.1 77329.50 9.02 0.139 0.127 0.027 1.22-0.95 350 336 39 8.6 49044.14 5.64 0.200 0.179 0.049 0.94-0.81 315 298 44 6.8 22889.50 3.34 0.137 0.120 0.071 0.81-0.73 261 249 42 5.9 26805.50 3.50 0.147 0.131 0.079 0.72-0.68 194 186 39 4.8 14418.94 2.24 0.134 0.143 0.101 0.67-0.63 167 155 39 4.0 17736.34 2.58 0.088 0.088 0.100 0.63-0.59 126 120 39 3.1 10857.68 1.96 0.098 0.095 0.126 0.59-0.56 97 95 40 2.4 10495.50 2.02 0.137 0.147 0.120 0.55-0.51 68 68 39 1.7 9274.59 2.05 0.124 0.136 0.128 0.51-0.46 32 32 29 1.1 7939.39 2.09 0.272 0.272 0.116 ------------------------------------------------------------------------------------------------------ inf-0.46 2031 1941 390 5.0 35897.33 4.55 0.151 0.135 0.052 inf-0.65 1629 1554 224 6.9 41733.50 5.13 0.154 0.138 0.047 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-1.26 402 40 40 100.0 10.1 77329.50 24.74 0.139 0.011 1.22-0.95 336 39 39 100.0 8.6 49044.14 14.23 0.200 0.023 0.94-0.81 298 44 44 100.0 6.8 22889.50 7.88 0.137 0.033 0.81-0.73 249 42 42 100.0 5.9 26805.50 8.04 0.147 0.039 0.72-0.68 186 39 39 100.0 4.8 14418.94 5.02 0.134 0.053 0.67-0.63 155 44 39 88.6 4.0 17736.34 4.80 0.088 0.058 0.63-0.59 120 45 39 86.7 3.1 10857.68 3.20 0.098 0.076 0.59-0.56 95 56 40 71.4 2.4 10495.50 3.00 0.137 0.074 0.55-0.51 68 85 39 45.9 1.7 9274.59 2.68 0.124 0.105 0.51-0.46 32 170 29 17.1 1.1 7939.39 2.12 0.272 0.976 -------------------------------------------------------------------------------------------- inf-0.46 1941 605 390 64.5 5.0 35897.33 11.17 0.151 0.029 inf-0.65 1554 225 224 99.6 6.9 41733.50 13.08 0.154 0.023 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 No constraint UB - matrix: 0.012563 -0.008713 -0.066474 ( 0.000021 0.000017 0.000015 ) 0.065075 -0.013421 0.014210 ( 0.000021 0.000018 0.000015 ) -0.014729 -0.066249 0.006040 ( 0.000028 0.000024 0.000021 ) M - matrix: 0.004610 -0.000007 0.000001 ( 0.000003 0.000002 0.000002 ) -0.000007 0.004645 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000012 0.004657 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.012563 -0.008713 -0.066474 ( 0.000021 0.000017 0.000015 ) 0.065075 -0.013421 0.014210 ( 0.000021 0.000018 0.000015 ) -0.014729 -0.066249 0.006040 ( 0.000028 0.000024 0.000021 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) unit cell: 10.447(3) 10.407(3) 10.394(3) 89.86(2) 90.01(2) 89.91(3) V = 1130.1(6) unit cell: 10.4160(8) 10.4160(8) 10.4160(8) 90.0 90.0 90.0 V = 1130.08(15) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.107) Run 2 Omega scan: (-49.000 - 51.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-552.0000 max=7876303.0000 PROFFIT INFO: signal sum lp corr: min=-608.8097 max=1117577.7511 PROFFIT INFO: background sum: min=130.0000 max=7706.0000 PROFFIT INFO: background sum sig2: min=387.0000 max=5044.0000 PROFFIT INFO: num of signal pixels: min=39 max=502 PROFFIT INFO: Inet: min=-974.0956 max=1788124.3750 PROFFIT INFO: sig(Inet): min=64.6188 max=24252.3379 PROFFIT INFO: Inet/sig(Inet): min=-1.59 max=180.79 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 372 1428 2108 2538 2728 3162 3426 3578 3846 4024 4062 Percent 9.2 35.2 51.9 62.5 67.2 77.8 84.3 88.1 94.7 99.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2031 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 2031 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1788124- 132318 203 397751.49 75.62 100.00 132268- 4086 203 30356.94 20.03 100.00 4070- 2114 203 2890.18 7.18 98.03 2113- 1255 203 1624.06 3.93 51.23 1253- 824 203 1029.42 2.18 11.82 819- 552 203 676.86 1.63 5.91 549- 324 203 431.48 1.30 7.88 323- 146 203 227.41 0.66 0.49 145- 9 203 75.28 0.27 0.00 8- -974 204 -143.36 -0.27 0.00 ------------------------------------------------------------------------------------ 1788124- -974 2031 43470.49 11.25 37.52 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 203 102772.81 14.82 69.95 1.64- 1.26 203 81715.47 20.82 58.13 1.26- 1.06 203 59495.78 18.43 67.98 1.06- 0.97 203 51463.21 14.35 29.56 0.97- 0.88 203 24594.75 8.60 45.32 0.88- 0.80 203 42615.90 12.12 34.48 0.80- 0.74 203 21769.65 6.67 22.66 0.74- 0.71 203 22571.52 7.17 16.26 0.71- 0.67 203 23597.32 7.50 24.63 0.67- 0.63 204 4301.48 2.02 6.37 ------------------------------------------------------------------------------------ 6.00- 0.63 2031 43470.49 11.25 37.52 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:48:56 2019 Sorting 2031 observations 41 unique observations with > 7.00 F2/sig(F2) 2031 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 98 202 Total number of frames 202 Maximum number of 41 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2031 observations in 2 runs Run # start # end # total # 1 0 20 21 2 0 19 41 Total number of frames 41 489 observations > 7.00 F2/sig(F2) 489 observations in 2 runs Run # start # end # total # 1 0 20 21 2 0 19 41 Total number of frames 41 Removing 'redundancy=1' reflections Average redundancy: 10.3 (Out of 489 removed 6 = 483, unique = 47) 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 483 observations in 2 runs Run # start # end # total # 1 0 20 21 2 0 19 41 Total number of frames 41 47 unique data precomputed (should be 47) 47 unique data with 483 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 10.3 (Out of 483 removed 0 = 483, unique = 47) 47 unique data precomputed (should be 47) 47 unique data with 483 observations RMS deviation of equivalent data = 0.23801 Rint = 0.20080 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19869, wR= 0.26208 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08673, wR= 0.15134, Acormin=0.611, Acormax=1.294, Acor_av=1.020 F test: Probability=1.000, F= 5.188 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10709, wR= 0.15256, Acormin=0.415, Acormax=1.381, Acor_av=0.890 F test: Probability=0.000, F= 0.651 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08313, wR= 0.14207, Acormin=0.510, Acormax=1.328, Acor_av=0.946 F test: Probability=0.744, F= 1.066 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08892, wR= 0.13055, Acormin=0.265, Acormax=1.463, Acor_av=0.807 F test: Probability=0.000, F= 0.925 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10189, wR= 0.14485, Acormin=0.208, Acormax=1.167, Acor_av=0.609 F test: Probability=0.000, F= 0.692 Final absorption model (ne=2, no=0): Rint= 0.08673, Acormin=0.611, Acormax=1.294, Acor_av=1.020 Combined refinement in use Rint: 0.20291 There are 41 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 45 pars with 1035 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.23801 Using Levenberg-Marquardt: 0.00010 New wR= 0.11144 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.08300 Rint for all data: 0.20291 with corrections 0.08611 0 observations identified as outliers and rejected Cycle 2 wR= 0.11144 Using Levenberg-Marquardt: 0.00001 New wR= 0.10845 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.07793 Rint for all data: 0.20291 with corrections 0.08109 0 observations identified as outliers and rejected Cycle 3 wR= 0.10845 Using Levenberg-Marquardt: 0.00000 New wR= 0.10751 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.07732 Rint for all data: 0.20291 with corrections 0.08048 0 observations identified as outliers and rejected Cycle 4 wR= 0.10751 Using Levenberg-Marquardt: 0.00000 New wR= 0.10692 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.07690 Rint for all data: 0.20291 with corrections 0.08006 1 observations identified as outliers and rejected Cycle 5 wR= 0.10025 Using Levenberg-Marquardt: 0.00000 New wR= 0.09970 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19925 with corrections 0.07388 Rint for all data: 0.20291 with corrections 0.07862 1 observations identified as outliers and rejected Final wR= 0.09970 Final frame scales: Min= 0.7298 Max= 1.2501 Final absorption correction factors: Amin= 0.6725 Amax= 1.3659 PROFFIT INFO: Inet (after scale3 abspack): min=-1101.0913 max=1228341.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=60.8545 max=22903.8184 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/103 2031 reflections read from tmp file 111 reflections are rejected (108 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 9 13 6 4 5 11 7 17 87 Initial Chi^2= 0.58891 Cycle 1, Chi^2= 1.03601 Current error model SIG(F2)^2 = 89.18*I_RAW + 4.84*I_BACK+(0.03488*)^2 Cycle 2, Chi^2= 1.02410 Current error model SIG(F2)^2 = 106.56*I_RAW + 2.89*I_BACK+(0.02532*)^2 Cycle 3, Chi^2= 1.00187 Current error model SIG(F2)^2 = 109.02*I_RAW + 2.77*I_BACK+(0.02627*)^2 Cycle 4, Chi^2= 1.00102 Current error model SIG(F2)^2 = 109.65*I_RAW + 2.69*I_BACK+(0.02611*)^2 Cycle 5, Chi^2= 1.00010 Current error model SIG(F2)^2 = 109.78*I_RAW + 2.69*I_BACK+(0.02614*)^2 Final Chi^2= 1.00010 Final error model SIG(F2)^2 = 109.78*I_RAW + 2.69*I_BACK+(0.02614*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1228341- 126105 203 379184.26 29.69 100.00 125204- 3843 203 30678.64 12.11 100.00 3826- 2050 203 2807.37 5.44 97.54 2048- 1207 203 1548.23 3.53 52.22 1206- 794 203 978.61 2.49 15.27 792- 520 203 669.60 2.12 9.36 520- 321 203 415.57 1.89 8.87 321- 144 203 223.57 1.35 1.48 144- 8 203 75.49 0.69 0.00 7- -1101 204 -146.32 -0.59 0.00 ------------------------------------------------------------------------------------ 1228341- -1101 2031 41622.93 5.87 38.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 203 98268.57 9.51 71.43 1.64- 1.26 203 77836.39 8.83 58.13 1.26- 1.06 203 60071.54 8.00 69.95 1.06- 0.97 203 48247.13 6.03 30.54 0.97- 0.88 203 21605.17 5.01 46.80 0.88- 0.80 203 42147.72 6.29 34.98 0.80- 0.74 203 21318.75 4.06 21.67 0.74- 0.71 203 20133.00 4.58 17.73 0.71- 0.67 203 22411.46 4.66 26.11 0.67- 0.63 204 4373.02 1.73 7.35 ------------------------------------------------------------------------------------ 6.00- 0.63 2031 41622.93 5.87 38.45 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 203 98268.57 9.51 71.43 6.00- 1.26 406 88052.48 9.17 64.78 6.00- 1.06 609 78725.50 8.78 66.50 6.00- 0.97 812 71105.91 8.09 57.51 6.00- 0.88 1015 61205.76 7.47 55.37 6.00- 0.80 1218 58029.42 7.28 51.97 6.00- 0.74 1421 52785.04 6.82 47.64 6.00- 0.71 1624 48703.53 6.54 43.90 6.00- 0.67 1827 45782.19 6.33 41.93 6.00- 0.63 2031 41622.93 5.87 38.45 ------------------------------------------------------------------------------------ 6.00- 0.63 2031 41622.93 5.87 38.45 Scale applied to data: s=0.814105 (maximum obs:1228341.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.079; Rsigma 0.039: data 2031 -> merged 162 With outlier rejection... Rint 0.065; Rsigma 0.040: data 2013 -> merged 162 Rejected total: 18, method kkm 15, method Blessing 3 Completeness direct cell (a, b, c) = (10.416, 10.416, 10.416), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626972, 6.013704 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.76 14 14 12.71 100.00 178 1.74 - 1.27 14 14 14.50 100.00 203 1.26 - 1.06 14 14 16.36 100.00 229 1.05 - 0.97 14 14 14.07 100.00 197 0.95 - 0.88 14 14 15.07 100.00 211 0.87 - 0.81 14 14 13.07 100.00 183 0.80 - 0.76 14 14 13.79 100.00 193 0.76 - 0.72 14 14 12.14 100.00 170 0.72 - 0.69 14 14 12.21 100.00 171 0.69 - 0.65 19 19 10.79 100.00 205 --------------------------------------------------------------- 7.37 - 0.65 145 145 13.38 100.00 1940 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:48:56 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.372177 7.367920 7.382795 120.2911 120.1112 89.6484 1941 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 990 974 974 979 1469 1292 1296 1941 N (int>3sigma) = 0 110 109 151 107 185 286 291 424 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 24.0 27.3 25.5 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.2 4.9 4.6 Lattice type: P chosen Volume: 282.70 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.343 7.365 7.368 119.96 119.75 90.10 Niggli form: a.a = 53.918 b.b = 54.245 c.c = 54.286 b.c = -27.104 a.c = -26.849 a.b = -0.097 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.419 CUBIC F-lattice R(int) = 0.211 [ 1705] Vol = 1130.8 Cell: 10.455 10.409 10.391 89.83 90.03 89.90 Volume: 1130.80 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.532 TETRAGONAL I-lattice R(int) = 0.157 [ 1356] Vol = 565.4 Cell: 7.370 7.383 10.391 90.10 89.85 89.75 Volume: 565.40 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.386 TETRAGONAL I-lattice R(int) = 0.200 [ 1353] Vol = 565.4 Cell: 7.343 7.365 10.455 90.04 89.91 90.10 Volume: 565.40 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.206 TETRAGONAL I-lattice R(int) = 0.157 [ 1356] Vol = 565.4 Cell: 7.383 7.370 10.391 90.15 90.10 90.25 Volume: 565.40 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.439 ORTHORHOMBIC F-lattice R(int) = 0.165 [ 1331] Vol = 1130.8 Cell: 10.391 10.409 10.455 89.90 90.03 89.83 Volume: 1130.80 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.546 ORTHORHOMBIC I-lattice R(int) = 0.128 [ 1305] Vol = 565.4 Cell: 10.391 7.383 7.370 89.75 89.85 90.10 Volume: 565.40 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.148 ORTHORHOMBIC I-lattice R(int) = 0.201 [ 1312] Vol = 565.4 Cell: 7.343 7.365 10.455 89.96 90.09 90.10 Volume: 565.40 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.355 MONOCLINIC I-lattice R(int) = 0.094 [ 911] Vol = 565.4 Cell: 7.370 10.391 7.383 90.10 90.25 90.15 Volume: 565.40 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.378 MONOCLINIC I-lattice R(int) = 0.160 [ 995] Vol = 565.4 Cell: 7.368 10.409 7.372 89.95 90.35 89.81 Volume: 565.40 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.340 MONOCLINIC I-lattice R(int) = 0.094 [ 911] Vol = 565.4 Cell: 7.383 10.391 7.370 90.15 90.25 90.10 Volume: 565.40 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.099 MONOCLINIC I-lattice R(int) = 0.189 [ 994] Vol = 565.4 Cell: 7.343 7.365 10.455 90.04 90.09 89.90 Volume: 565.40 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.068 MONOCLINIC I-lattice R(int) = 0.155 [ 896] Vol = 565.4 Cell: 7.343 10.455 7.365 90.04 90.10 89.91 Volume: 565.40 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.125 MONOCLINIC I-lattice R(int) = 0.155 [ 896] Vol = 565.4 Cell: 7.343 10.455 7.365 89.96 90.10 90.09 Volume: 565.40 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.082 [ 371] Vol = 282.7 Cell: 7.343 7.365 7.368 119.96 119.75 90.10 Volume: 282.70 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 0 974 0 1285 1299 1941 N (int>3sigma) = 0 0 0 0 151 0 293 296 424 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 26.8 25.3 25.5 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.6 4.6 4.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.770 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 12 12 147 360 N I>3s 0 0 0 91 0.1 0.1 -0.0 1.7 0.8 0.8 0.1 2.6 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 0.211 1586 Fd-3m 1 1 227 C N N N N 37 2284 0.213 1649 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.454754 10.409449 10.390794 89.8271 90.0331 89.9041 ZERR 1.00 0.001250 0.013299 0.007175 0.0000 0.0006 0.1373 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1098048- 99209 245 234 27 8.7 330126.63 27.84 0.060 0.066 86569- 1697 392 386 27 14.3 5214.45 7.31 0.104 0.094 1627- 844 386 385 27 14.3 1166.65 2.74 0.248 0.304 788- 366 360 360 27 13.3 546.09 1.93 0.378 0.464 359- 63 354 354 27 13.1 226.57 1.17 0.584 0.928 54- -344 294 294 27 10.9 -4.42 0.13 0.971 3.650 ------------------------------------------------------------------------------------------- 1098048- -344 2031 2013 162 12.4 39735.25 5.73 0.065 0.069 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-1.27 386 379 27 14.0 87253.36 9.28 0.056 0.059 0.030 1.26-0.97 429 426 28 15.2 49472.13 6.58 0.065 0.076 0.036 0.95-0.81 388 385 27 14.3 32578.02 5.76 0.076 0.086 0.046 0.81-0.73 354 352 27 13.0 15158.99 3.47 0.059 0.056 0.062 0.73-0.67 311 310 28 11.1 23422.94 4.82 0.082 0.100 0.062 0.66-0.63 163 161 25 6.4 4368.31 1.76 0.117 0.075 0.127 ------------------------------------------------------------------------------------------------------ inf-0.63 2031 2013 162 12.4 39735.25 5.73 0.065 0.069 0.040 inf-0.65 1954 1938 144 13.5 40991.49 5.87 0.064 0.069 0.039 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-1.27 379 27 27 100.0 14.0 87253.36 33.72 0.056 0.012 1.26-0.97 426 28 28 100.0 15.2 49472.13 24.57 0.065 0.012 0.95-0.81 385 27 27 100.0 14.3 32578.02 21.63 0.076 0.015 0.81-0.73 352 27 27 100.0 13.0 15158.99 11.65 0.059 0.020 0.73-0.67 310 28 28 100.0 11.1 23422.94 16.87 0.082 0.020 0.66-0.63 161 25 25 100.0 6.4 4368.31 4.51 0.117 0.053 -------------------------------------------------------------------------------------------- inf-0.63 2013 162 162 100.0 12.4 39735.25 20.68 0.065 0.014 inf-0.65 1938 144 144 100.0 13.5 40991.49 21.33 0.064 0.014 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:50:23 2019) ID: 3668; threads 39; handles 810; mem 515344.00 (1196496.00)kB; time: 1w 4d 23h 1m 11s MEMORY INFO: Memory PF:280.0, Ph:667.0, V:1168.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:503.3,peak PF: 700.2, WS: 471.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:282.0, Ph:668.0, V:1170.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:505.1,peak PF: 700.2, WS: 473.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:50:23 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000102 0.000065 0.000100 ) 0.064809 0.092374 0.027273 ( 0.000113 0.000072 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000133 0.000084 0.000130 ) 7.38096 ( 0.00738 ) 7.36649 ( 0.00769 ) 7.42630 ( 0.00865 ) 120.52449 ( 0.11716 ) 120.40327 ( 0.11455 ) 89.27095 ( 0.08278 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:50:23 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000102 0.000065 0.000100 ) 0.064809 0.092374 0.027273 ( 0.000113 0.000072 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000133 0.000084 0.000130 ) M - matrix: 0.013828 0.004569 0.009203 ( 0.000026 0.000016 0.000022 ) 0.004569 0.013978 0.009343 ( 0.000016 0.000017 0.000018 ) 0.009203 0.009343 0.018473 ( 0.000022 0.000018 0.000035 ) unit cell: 7.381(7) 7.366(8) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb PROFFITPEAK info: 518 peaks in the peak location table UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) 277 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-11.3 | 47 | 0.972 ( 0.040) | 1.005 ( 0.088) | 1.150 ( 0.463) | 11.3-15.2 | 47 | 1.023 ( 0.296) | 1.053 ( 0.090) | 1.390 ( 1.521) | 15.4-19.8 | 47 | 0.955 ( 0.058) | 1.008 ( 0.091) | 1.062 ( 0.500) | 19.9-24.0 | 47 | 0.950 ( 0.054) | 1.003 ( 0.089) | 0.904 ( 0.383) | 24.0-27.5 | 47 | 0.949 ( 0.069) | 0.992 ( 0.101) | 0.979 ( 0.458) | 27.6-33.1 | 47 | 0.928 ( 0.099) | 0.933 ( 0.113) | 0.944 ( 0.472) | 33.1-36.7 | 47 | 0.923 ( 0.207) | 0.890 ( 0.127) | 1.129 ( 0.768) | 36.7-39.1 | 47 | 0.856 ( 0.083) | 0.828 ( 0.114) | 1.008 ( 0.505) | 39.1-42.0 | 47 | 0.896 ( 0.091) | 0.835 ( 0.123) | 1.155 ( 0.490) | 42.0-50.1 | 43 | 0.861 ( 0.107) | 0.777 ( 0.118) | 1.032 ( 0.527) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 466 | 0.932 ( 0.143) | 0.934 ( 0.139) | 1.076 ( 0.701) | Fitted profile normalization line parameters e1 dimension: a=-0.0035 b=1.14 e2 dimension: a=-0.0078 b=1.27 e3 dimension: a=0.0050 b=0.93 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 12:50:31 2019 PROFFITMAIN - Started at Wed Aug 21 12:50:31 2019 OTKP changes: 256 2 1 2 OTKP changes: 256 2 1 2 OTKP changes: 256 2 1 2 UB - matrix: 0.087548 -0.046028 0.017103 ( 0.000096 0.000061 0.000095 ) 0.064103 0.092428 0.027178 ( 0.000104 0.000066 0.000102 ) 0.045416 0.057704 0.132145 ( 0.000112 0.000071 0.000110 ) M - matrix: 0.013836 0.004516 0.009241 ( 0.000024 0.000014 0.000019 ) 0.004516 0.013991 0.009350 ( 0.000014 0.000016 0.000015 ) 0.009241 0.009350 0.018493 ( 0.000019 0.000015 0.000030 ) UB fit with 276 obs out of 466 (total:466,skipped:0) (59.23%) unit cell: 7.388(7) 7.370(7) 7.429(7) 120.67(10) 120.36(10) 89.03(8) V = 284.0(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 202 obs out of 212 (total:212,skipped:0) (95.28%) UB - matrix: 0.087482 -0.046126 0.017387 ( 0.000099 0.000061 0.000092 ) 0.064752 0.092358 0.027241 ( 0.000086 0.000054 0.000080 ) 0.045708 0.057845 0.132152 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013935 0.004589 0.009325 ( 0.000023 0.000013 0.000018 ) 0.004589 0.014004 0.009358 ( 0.000013 0.000014 0.000013 ) 0.009325 0.009358 0.018509 ( 0.000018 0.000013 0.000026 ) unit cell: 7.381(6) 7.367(6) 7.434(6) 120.52(9) 120.47(9) 89.22(7) V = 283.5(4) OTKP changes: 200 1 1 1 OTKP changes: 200 1 1 1 OTKP changes: 200 1 1 1 UB - matrix: 0.087357 -0.045952 0.017474 ( 0.000098 0.000061 0.000092 ) 0.064664 0.092297 0.027268 ( 0.000086 0.000053 0.000081 ) 0.045527 0.057801 0.132003 ( 0.000102 0.000063 0.000096 ) M - matrix: 0.013885 0.004586 0.009299 ( 0.000022 0.000013 0.000017 ) 0.004586 0.013971 0.009344 ( 0.000013 0.000013 0.000013 ) 0.009299 0.009344 0.018474 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.394(6) 7.377(6) 7.441(6) 120.52(9) 120.44(9) 89.27(7) V = 284.6(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.108) HKL list info: 1300 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087357 -0.045952 0.017474 ( 0.000098 0.000061 0.000092 ) 0.064664 0.092297 0.027268 ( 0.000086 0.000053 0.000081 ) 0.045526 0.057801 0.132003 ( 0.000102 0.000064 0.000096 ) M - matrix: 0.013885 0.004585 0.009299 ( 0.000022 0.000013 0.000017 ) 0.004585 0.013971 0.009344 ( 0.000013 0.000013 0.000013 ) 0.009299 0.009344 0.018474 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.394(6) 7.377(6) 7.441(6) 120.52(9) 120.44(9) 89.27(7) V = 284.6(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118029 0.039095 0.078775 ( 0.000075 0.000047 0.000069 ) 0.000036 0.111506 0.056219 ( 0.000075 0.000047 0.000070 ) 0.000027 -0.000046 0.095480 ( 0.000090 0.000056 0.000084 ) M - matrix: 0.013931 0.004618 0.009302 ( 0.000018 0.000010 0.000014 ) 0.004618 0.013962 0.009344 ( 0.000010 0.000011 0.000011 ) 0.009302 0.009344 0.018483 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.376(5) 7.380(5) 7.428(8) 120.46(9) 120.29(9) 89.48(5) V = 284.0(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117847 0.039064 0.078712 ( 0.000038 0.000033 0.000040 ) -0.000016 0.111485 0.056239 ( 0.000037 0.000033 0.000039 ) 0.000004 -0.000147 0.096021 ( 0.000047 0.000041 0.000049 ) M - matrix: 0.013888 0.004602 0.009276 ( 0.000009 0.000006 0.000007 ) 0.004602 0.013955 0.009330 ( 0.000006 0.000008 0.000007 ) 0.009276 0.009330 0.018578 ( 0.000007 0.000007 0.000012 ) UB fit with 461 obs out of 466 (total:466,skipped:0) (98.93%) unit cell: 7.372(3) 7.368(3) 7.381(4) 120.29(5) 120.11(5) 89.65(3) V = 282.6(2) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 64 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof 2064 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:50:34 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.108) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-552.0000 max=7905610.0000 PROFFIT INFO: signal sum lp corr: min=-608.8090 max=1126218.4216 PROFFIT INFO: background sum: min=131.0000 max=7559.0000 PROFFIT INFO: background sum sig2: min=396.0000 max=5054.0000 PROFFIT INFO: num of signal pixels: min=39 max=503 PROFFIT INFO: Inet: min=-974.0944 max=1801949.3750 PROFFIT INFO: sig(Inet): min=64.6191 max=24251.6211 PROFFIT INFO: Inet/sig(Inet): min=-1.59 max=180.88 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 193 726 1075 1291 1391 1611 1743 1820 1955 2045 2064 Percent 9.4 35.2 52.1 62.5 67.4 78.1 84.4 88.2 94.7 99.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2064 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 2064 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1801949- 132272 206 394469.59 75.41 100.00 131455- 3981 206 29375.69 19.78 100.00 3976- 2084 206 2861.21 7.07 98.06 2076- 1255 206 1607.81 3.88 50.00 1249- 826 206 1023.81 2.17 11.17 824- 552 206 676.98 1.63 6.31 548- 330 206 437.94 1.32 8.74 328- 143 206 229.61 0.66 0.97 143- 8 206 73.70 0.26 0.00 6- -974 210 -140.14 -0.27 0.00 ------------------------------------------------------------------------------------ 1801949- -974 2064 42977.90 11.17 37.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 206 93349.05 15.48 67.48 1.75- 1.28 206 90302.26 21.02 58.74 1.28- 1.06 206 48957.48 13.48 50.00 1.06- 0.93 206 35381.66 11.44 43.69 0.93- 0.84 206 42860.57 12.41 31.55 0.84- 0.76 206 30923.85 9.85 33.01 0.76- 0.71 206 32054.45 9.62 31.55 0.71- 0.65 206 17276.82 5.87 19.90 0.65- 0.59 206 24054.85 7.56 23.30 0.59- 0.46 210 15158.15 5.07 15.71 ------------------------------------------------------------------------------------ 6.55- 0.46 2064 42977.90 11.17 37.45 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:50:35 2019 Sorting 2064 observations 69 unique observations with > 7.00 F2/sig(F2) 2064 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 102 206 Total number of frames 206 Maximum number of 69 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 2064 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 34 70 Total number of frames 70 491 observations > 7.00 F2/sig(F2) 491 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 33 69 Total number of frames 69 Removing 'redundancy=1' reflections Average redundancy: 4.7 (Out of 491 removed 39 = 452, unique = 97) 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 452 observations in 2 runs Run # start # end # total # 1 0 34 35 2 0 33 69 Total number of frames 69 97 unique data precomputed (should be 97) 97 unique data with 452 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.7 (Out of 452 removed 0 = 452, unique = 97) 97 unique data precomputed (should be 97) 97 unique data with 452 observations RMS deviation of equivalent data = 0.37571 Rint = 0.35289 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.35289, wR= 0.47249 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26716, wR= 0.35771, Acormin=0.349, Acormax=1.456, Acor_av=0.836 F test: Probability=1.000, F= 1.720 Trying model 2 (ne=2, no=1)... Results: Rint= 0.30928, wR= 0.38050, Acormin=0.084, Acormax=1.635, Acor_av=0.609 F test: Probability=0.000, F= 0.740 Trying model 3 (ne=4, no=0)... Results: Rint= 0.28637, wR= 0.32338, Acormin=0.067, Acormax=1.914, Acor_av=0.707 F test: Probability=0.000, F= 0.848 Trying model 4 (ne=4, no=1)... Results: Rint= 0.32374, wR= 0.33879, Acormin=0.003, Acormax=1.684, Acor_av=0.517 F test: Probability=0.000, F= 0.658 Trying model 5 (ne=4, no=3)... Results: Rint= 0.34246, wR= 0.34051, Acormin=-0.087, Acormax=1.846, Acor_av=0.352 F test: Probability=0.000, F= 0.576 Trying model 6 (ne=6, no=0)... Results: Rint= 0.28067, wR= 0.32489, Acormin=-0.097, Acormax=1.678, Acor_av=0.596 F test: Probability=0.000, F= 0.849 Trying model 7 (ne=6, no=1)... Results: Rint= 0.31773, wR= 0.33737, Acormin=0.028, Acormax=1.456, Acor_av=0.481 F test: Probability=0.000, F= 0.657 Trying model 8 (ne=6, no=3)... Results: Rint= 0.29416, wR= 0.31243, Acormin=-0.195, Acormax=1.969, Acor_av=0.359 F test: Probability=0.000, F= 0.749 Trying model 9 (ne=6, no=5)... Results: Rint= 0.27229, wR= 0.32383, Acormin=-0.106, Acormax=2.583, Acor_av=0.174 F test: Probability=0.000, F= 0.844 Trying model 10 (ne=8, no=0)... Results: Rint= 0.30902, wR= 0.36430, Acormin=-0.172, Acormax=1.842, Acor_av=0.433 F test: Probability=0.000, F= 0.664 Trying model 11 (ne=8, no=1)... Results: Rint= 0.40388, wR= 0.43262, Acormin=-0.098, Acormax=1.052, Acor_av=0.269 F test: Probability=0.000, F= 0.385 Trying model 12 (ne=8, no=3)... Results: Rint= 0.20401, wR= 0.23315, Acormin=-0.017, Acormax=0.188, Acor_av=0.058 F test: Probability=1.000, F= 1.475 Trying model 13 (ne=8, no=5)... Results: Rint= 0.18499, wR= 0.20607, Acormin=-0.008, Acormax=0.211, Acor_av=0.066 F test: Probability=1.000, F= 1.728 Trying model 14 (ne=8, no=7)... Results: Rint= 0.13166, wR= 0.17374, Acormin=0.010, Acormax=0.265, Acor_av=0.079 F test: Probability=1.000, F= 3.235 Final absorption model (ne=2, no=0): Rint= 0.26716, Acormin=0.349, Acormax=1.456, Acor_av=0.836 Combined refinement in use Rint: 0.36775 There are 69 active scales (one needs to be fixed) Refinement control: frame scale #37 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= 0.37571 Using Levenberg-Marquardt: 0.00010 New wR= 0.20786 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35289 with corrections 0.18091 Rint for all data: 0.36775 with corrections 0.19793 0 observations identified as outliers and rejected Cycle 2 wR= 0.20786 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= 0.88114 Using Levenberg-Marquardt: 0.01000 New wR= 0.23344 Using Levenberg-Marquardt: 0.10000 New wR= 0.18843 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35289 with corrections 0.16294 Rint for all data: 0.36775 with corrections 0.18026 0 observations identified as outliers and rejected Cycle 3 wR= 0.18843 Using Levenberg-Marquardt: 0.01000 New wR= 0.18321 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35289 with corrections 0.16032 Rint for all data: 0.36775 with corrections 0.17770 0 observations identified as outliers and rejected Cycle 4 wR= 0.18321 Using Levenberg-Marquardt: 0.00100 New wR= 0.17976 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35289 with corrections 0.15836 Rint for all data: 0.36775 with corrections 0.17579 0 observations identified as outliers and rejected Cycle 5 wR= 0.17976 Using Levenberg-Marquardt: 0.00010 New wR= 0.17741 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35289 with corrections 0.15719 Rint for all data: 0.36775 with corrections 0.17458 0 observations identified as outliers and rejected Final wR= 0.17741 Final frame scales: Min= 0.3491 Max= 1.3267 Final absorption correction factors: Amin= 0.4258 Amax= 1.3395 PROFFIT INFO: Inet (after scale3 abspack): min=-1579.4092 max=1444503.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=41.3356 max=26319.4102 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/103 2064 reflections read from tmp file 571 reflections are rejected (495 as outliers, 76 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 61 64 39 31 41 23 19 11 19 Initial Chi^2= 2.61034 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.70362 Current error model SIG(F2)^2 = 586.51*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 412.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 412.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1444503- 127075 206 354847.10 31.80 100.00 122066- 3897 206 26250.19 6.92 83.98 3888- 1937 206 2667.35 2.60 24.76 1934- 1167 206 1529.85 2.00 17.48 1167- 737 206 939.76 1.44 3.40 736- 486 206 616.22 1.12 0.49 485- 285 206 386.34 1.05 0.49 285- 133 206 211.28 0.88 1.94 132- 6 206 67.33 0.46 0.00 6- -1579 210 -168.77 -0.34 0.00 ------------------------------------------------------------------------------------ 1444503- -1579 2064 38659.27 4.78 23.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 206 87103.78 10.38 51.46 1.75- 1.28 206 86031.56 8.97 40.78 1.28- 1.06 206 42497.60 5.83 29.61 1.06- 0.93 206 40531.67 4.15 19.90 0.93- 0.84 206 35240.31 4.40 19.42 0.84- 0.76 206 29649.72 3.59 16.99 0.76- 0.71 206 25755.06 3.48 17.96 0.71- 0.65 206 12343.40 2.30 8.25 0.65- 0.59 206 18652.62 2.84 16.99 0.59- 0.46 210 9355.98 1.97 10.95 ------------------------------------------------------------------------------------ 6.55- 0.46 2064 38659.27 4.78 23.21 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 206 87103.78 10.38 51.46 6.55- 1.28 412 86567.67 9.68 46.12 6.55- 1.06 618 71877.65 8.39 40.61 6.55- 0.93 824 64041.15 7.33 35.44 6.55- 0.84 1030 58280.98 6.75 32.23 6.55- 0.76 1236 53509.11 6.22 29.69 6.55- 0.71 1442 49544.24 5.83 28.02 6.55- 0.65 1648 44894.14 5.39 25.55 6.55- 0.59 1854 41978.41 5.10 24.60 6.55- 0.46 2064 38659.27 4.78 23.21 ------------------------------------------------------------------------------------ 6.55- 0.46 2064 38659.27 4.78 23.21 Scale applied to data: s=0.692279 (maximum obs:1444503.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.175; Rsigma 0.051: data 2064 -> merged 390 With outlier rejection... Rint 0.141; Rsigma 0.052: data 1970 -> merged 390 Rejected total: 94, method kkm 88, method Blessing 6 Completeness direct cell (a, b, c) = (6.563, 6.563, 6.563), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.457243, 6.562673 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.59 22 22 10.50 100.00 231 1.55 - 1.22 22 22 9.95 100.00 219 1.20 - 1.02 22 22 9.23 100.00 203 1.02 - 0.92 22 22 7.73 100.00 170 0.92 - 0.84 22 22 7.50 100.00 165 0.84 - 0.79 22 22 6.05 100.00 133 0.79 - 0.75 22 22 5.91 100.00 130 0.75 - 0.71 22 22 4.77 100.00 105 0.71 - 0.69 22 22 4.91 100.00 108 0.68 - 0.65 26 29 4.58 89.66 119 --------------------------------------------------------------- 7.37 - 0.65 224 227 7.07 98.68 1583 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:50:35 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.372270 7.367551 7.381422 120.2866 120.1130 89.6500 1970 Reflections read from file xs2212a.hkl 1970 Reflections used for space-group determination (up to diffraction limit of 0.46A); mean (I/sigma) = 4.50 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1001 993 988 992 1491 1308 1311 1970 N (int>3sigma) = 0 112 112 150 107 187 285 293 428 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 23.2 26.7 24.6 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.2 4.9 4.5 Lattice type: P chosen Volume: 282.65 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.343 7.364 7.368 119.96 119.76 90.09 Niggli form: a.a = 53.913 b.b = 54.232 c.c = 54.281 b.c = -27.095 a.c = -26.854 a.b = -0.089 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.406 CUBIC F-lattice R(int) = 0.209 [ 1734] Vol = 1130.6 Cell: 10.454 10.408 10.391 89.83 90.04 89.91 Volume: 1130.58 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.524 TETRAGONAL I-lattice R(int) = 0.162 [ 1385] Vol = 565.3 Cell: 7.370 7.381 10.391 90.09 89.85 89.74 Volume: 565.29 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.374 TETRAGONAL I-lattice R(int) = 0.195 [ 1381] Vol = 565.3 Cell: 7.343 7.364 10.454 90.03 89.91 90.09 Volume: 565.29 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.216 TETRAGONAL I-lattice R(int) = 0.162 [ 1385] Vol = 565.3 Cell: 7.381 7.370 10.391 90.15 90.09 90.26 Volume: 565.29 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.420 ORTHORHOMBIC F-lattice R(int) = 0.160 [ 1359] Vol = 1130.6 Cell: 10.391 10.408 10.454 89.91 90.04 89.83 Volume: 1130.58 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.543 ORTHORHOMBIC I-lattice R(int) = 0.124 [ 1334] Vol = 565.3 Cell: 10.391 7.381 7.370 89.74 89.85 90.09 Volume: 565.29 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.137 ORTHORHOMBIC I-lattice R(int) = 0.201 [ 1341] Vol = 565.3 Cell: 7.343 7.364 10.454 89.97 90.09 90.09 Volume: 565.29 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.349 MONOCLINIC I-lattice R(int) = 0.087 [ 938] Vol = 565.3 Cell: 7.370 10.391 7.381 90.09 90.26 90.15 Volume: 565.29 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.367 MONOCLINIC I-lattice R(int) = 0.155 [ 1016] Vol = 565.3 Cell: 7.368 10.408 7.372 89.94 90.35 89.82 Volume: 565.29 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.332 MONOCLINIC I-lattice R(int) = 0.087 [ 938] Vol = 565.3 Cell: 7.381 10.391 7.370 90.15 90.26 90.09 Volume: 565.29 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.091 MONOCLINIC I-lattice R(int) = 0.188 [ 1023] Vol = 565.3 Cell: 7.343 7.364 10.454 90.03 90.09 89.91 Volume: 565.29 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.062 MONOCLINIC I-lattice R(int) = 0.149 [ 921] Vol = 565.3 Cell: 7.343 10.454 7.364 90.03 90.09 89.91 Volume: 565.29 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.122 MONOCLINIC I-lattice R(int) = 0.149 [ 921] Vol = 565.3 Cell: 7.343 10.454 7.364 89.97 90.09 90.09 Volume: 565.29 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.077 [ 383] Vol = 282.6 Cell: 7.343 7.364 7.368 119.96 119.76 90.09 Volume: 282.65 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 0 988 0 1305 1314 1970 N (int>3sigma) = 0 0 0 0 150 0 297 300 428 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 25.3 24.7 24.6 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.5 4.6 4.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.815 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 12 12 151 368 N I>3s 0 0 1 90 0.1 0.1 -0.0 1.6 0.7 0.7 0.1 2.5 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 0.209 1611 Fd-3m 1 1 227 C N N N N 37 2284 0.209 1674 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.454413 10.407790 10.390745 89.8308 90.0367 89.9145 ZERR 1.00 0.001215 0.012944 0.006976 0.0002 0.0002 0.1340 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 900361- 117369 219 194 39 5.0 337331.50 30.52 0.122 0.116 109380- 2739 231 218 39 5.6 14825.24 4.73 0.272 0.152 2737- 1493 355 338 39 8.7 1949.22 2.15 0.799 0.897 1490- 1065 270 257 39 6.6 1118.71 1.42 0.686 0.730 1051- 823 213 210 39 5.4 885.99 1.25 0.703 0.699 822- 622 179 172 39 4.4 649.31 1.02 0.678 0.715 619- 480 199 191 39 4.9 491.12 0.79 0.735 0.885 470- 351 146 142 39 3.6 384.05 0.77 0.639 0.789 349- 133 149 146 39 3.7 250.34 0.66 0.735 0.883 127- -980 103 102 39 2.6 38.12 0.21 0.920 2.641 ------------------------------------------------------------------------------------------- 900361- -980 2064 1970 390 5.1 35587.35 4.50 0.141 0.130 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-1.26 432 411 40 10.3 74565.24 8.70 0.137 0.128 0.028 1.22-0.95 356 347 39 8.9 48444.78 5.58 0.173 0.168 0.050 0.94-0.81 314 297 41 7.2 23462.57 3.33 0.141 0.118 0.070 0.81-0.73 243 227 39 5.8 26180.88 3.50 0.112 0.111 0.079 0.73-0.69 192 182 39 4.7 18640.21 2.58 0.120 0.114 0.090 0.68-0.64 174 166 39 4.3 17947.19 2.60 0.124 0.119 0.098 0.63-0.60 142 133 40 3.3 11471.34 2.02 0.097 0.095 0.124 0.59-0.56 102 98 40 2.5 9645.95 1.87 0.115 0.114 0.121 0.56-0.52 69 69 39 1.8 9164.60 2.03 0.109 0.125 0.128 0.52-0.46 40 40 34 1.2 6597.07 1.80 0.495 0.575 0.128 ------------------------------------------------------------------------------------------------------ inf-0.46 2064 1970 390 5.1 35587.35 4.50 0.141 0.130 0.052 inf-0.65 1662 1583 224 7.1 41014.74 5.03 0.143 0.131 0.048 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-1.26 411 40 40 100.0 10.3 74565.24 23.99 0.137 0.011 1.22-0.95 347 39 39 100.0 8.9 48444.78 14.08 0.173 0.022 0.94-0.81 297 41 41 100.0 7.2 23462.57 7.95 0.141 0.031 0.81-0.73 227 39 39 100.0 5.8 26180.88 8.03 0.112 0.041 0.73-0.69 182 39 39 100.0 4.7 18640.21 5.57 0.120 0.047 0.68-0.64 166 43 39 90.7 4.3 17947.19 5.23 0.124 0.055 0.63-0.60 133 44 40 90.9 3.3 11471.34 3.19 0.097 0.074 0.59-0.56 98 57 40 70.2 2.5 9645.95 2.81 0.115 0.073 0.56-0.52 69 75 39 52.0 1.8 9164.60 2.67 0.109 0.109 0.52-0.46 40 190 34 17.9 1.2 6597.07 1.81 0.495 1.232 -------------------------------------------------------------------------------------------- inf-0.46 1970 611 390 63.8 5.1 35587.35 11.05 0.141 0.030 inf-0.65 1583 225 224 99.6 7.1 41014.74 12.84 0.143 0.024 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 No constraint UB - matrix: 0.012566 -0.008720 -0.066472 ( 0.000020 0.000017 0.000015 ) 0.065074 -0.013405 0.014223 ( 0.000021 0.000017 0.000015 ) -0.014715 -0.066251 0.006037 ( 0.000028 0.000023 0.000021 ) M - matrix: 0.004609 -0.000007 0.000001 ( 0.000003 0.000002 0.000002 ) -0.000007 0.004645 -0.000011 ( 0.000002 0.000003 0.000002 ) 0.000001 -0.000011 0.004657 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.012566 -0.008720 -0.066472 ( 0.000020 0.000017 0.000015 ) 0.065074 -0.013405 0.014223 ( 0.000021 0.000017 0.000015 ) -0.014715 -0.066251 0.006037 ( 0.000028 0.000023 0.000021 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) unit cell: 10.448(3) 10.407(3) 10.394(3) 89.86(2) 90.02(2) 89.91(3) V = 1130.1(6) unit cell: 10.4162(8) 10.4162(8) 10.4162(8) 90.0 90.0 90.0 V = 1130.13(15) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.108) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-552.0000 max=7905610.0000 PROFFIT INFO: signal sum lp corr: min=-608.8090 max=1126218.4216 PROFFIT INFO: background sum: min=131.0000 max=7559.0000 PROFFIT INFO: background sum sig2: min=396.0000 max=5054.0000 PROFFIT INFO: num of signal pixels: min=39 max=503 PROFFIT INFO: Inet: min=-974.0944 max=1801949.3750 PROFFIT INFO: sig(Inet): min=64.6191 max=24251.6211 PROFFIT INFO: Inet/sig(Inet): min=-1.59 max=180.88 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 386 1452 2150 2582 2782 3222 3486 3640 3910 4090 4128 Percent 9.4 35.2 52.1 62.5 67.4 78.1 84.4 88.2 94.7 99.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2064 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 2064 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1801949- 132272 206 394469.59 75.41 100.00 131455- 3981 206 29375.69 19.78 100.00 3976- 2084 206 2861.21 7.07 98.06 2076- 1255 206 1607.81 3.88 50.00 1249- 826 206 1023.81 2.17 11.17 824- 552 206 676.98 1.63 6.31 548- 330 206 437.94 1.32 8.74 328- 143 206 229.61 0.66 0.97 143- 8 206 73.70 0.26 0.00 6- -974 210 -140.14 -0.27 0.00 ------------------------------------------------------------------------------------ 1801949- -974 2064 42977.90 11.17 37.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 206 101337.80 14.66 69.42 1.64- 1.26 206 80431.20 20.53 57.77 1.26- 1.06 206 65322.75 19.88 69.42 1.06- 0.97 206 44058.61 12.52 29.13 0.97- 0.88 206 27237.64 9.30 45.63 0.88- 0.80 206 40951.10 11.90 33.98 0.80- 0.75 206 20866.62 6.45 22.82 0.75- 0.71 206 22861.81 7.25 16.99 0.71- 0.67 206 23266.72 7.43 24.27 0.67- 0.63 210 4197.71 1.96 5.71 ------------------------------------------------------------------------------------ 6.00- 0.63 2064 42977.90 11.17 37.45 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:50:35 2019 Sorting 2064 observations 41 unique observations with > 7.00 F2/sig(F2) 2064 observations in 2 runs Run # start # end # total # 1 0 102 103 2 0 102 206 Total number of frames 206 Maximum number of 41 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 2064 observations in 2 runs Run # start # end # total # 1 0 17 18 2 0 17 36 Total number of frames 36 491 observations > 7.00 F2/sig(F2) 491 observations in 2 runs Run # start # end # total # 1 0 17 18 2 0 16 35 Total number of frames 35 Removing 'redundancy=1' reflections Average redundancy: 10.5 (Out of 491 removed 7 = 484, unique = 46) 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 484 observations in 2 runs Run # start # end # total # 1 0 17 18 2 0 16 35 Total number of frames 35 46 unique data precomputed (should be 46) 46 unique data with 484 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 10.5 (Out of 484 removed 0 = 484, unique = 46) 46 unique data precomputed (should be 46) 46 unique data with 484 observations RMS deviation of equivalent data = 0.23795 Rint = 0.20088 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19877, wR= 0.26217 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08770, wR= 0.15186, Acormin=0.611, Acormax=1.296, Acor_av=1.017 F test: Probability=1.000, F= 5.078 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10814, wR= 0.15233, Acormin=0.416, Acormax=1.376, Acor_av=0.891 F test: Probability=0.000, F= 0.653 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08594, wR= 0.14421, Acormin=0.495, Acormax=1.321, Acor_av=0.936 F test: Probability=0.580, F= 1.020 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09230, wR= 0.13297, Acormin=0.274, Acormax=1.451, Acor_av=0.798 F test: Probability=0.000, F= 0.878 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10326, wR= 0.14646, Acormin=0.209, Acormax=1.156, Acor_av=0.603 F test: Probability=0.000, F= 0.690 Final absorption model (ne=2, no=0): Rint= 0.08770, Acormin=0.611, Acormax=1.296, Acor_av=1.017 Combined refinement in use Rint: 0.20294 There are 35 active scales (one needs to be fixed) Refinement control: frame scale #32 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 39 pars with 780 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.23795 Using Levenberg-Marquardt: 0.00010 New wR= 0.12887 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.20088 with corrections 0.08219 Rint for all data: 0.20294 with corrections 0.08528 2 observations identified as outliers and rejected Cycle 2 wR= 0.10826 Using Levenberg-Marquardt: 0.00001 New wR= 0.10114 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19821 with corrections 0.06846 Rint for all data: 0.20294 with corrections 0.07570 2 observations identified as outliers and rejected Cycle 3 wR= 0.08684 Using Levenberg-Marquardt: 0.00000 New wR= 0.08226 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19506 with corrections 0.05940 Rint for all data: 0.20294 with corrections 0.07039 0 observations identified as outliers and rejected Cycle 4 wR= 0.08226 Using Levenberg-Marquardt: 0.00000 New wR= 0.08201 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19506 with corrections 0.05939 Rint for all data: 0.20294 with corrections 0.07044 1 observations identified as outliers and rejected Cycle 5 wR= 0.07809 Using Levenberg-Marquardt: 0.00000 New wR= 0.07777 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19614 with corrections 0.05763 Rint for all data: 0.20294 with corrections 0.07038 0 observations identified as outliers and rejected Final wR= 0.07777 Final frame scales: Min= 0.8542 Max= 1.2431 Final absorption correction factors: Amin= 0.6771 Amax= 1.4012 PROFFIT INFO: Inet (after scale3 abspack): min=-1027.3386 max=1180812.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=59.2021 max=23789.6465 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/103 2064 reflections read from tmp file 96 reflections are rejected (93 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 11 9 8 1 9 7 8 11 95 Initial Chi^2= 0.55249 Cycle 1, Chi^2= 1.02678 Current error model SIG(F2)^2 = 81.77*I_RAW + 6.18*I_BACK+(0.02941*)^2 Cycle 2, Chi^2= 1.02025 Current error model SIG(F2)^2 = 95.27*I_RAW + 4.16*I_BACK+(0.02354*)^2 Cycle 3, Chi^2= 1.00122 Current error model SIG(F2)^2 = 96.45*I_RAW + 4.06*I_BACK+(0.02502*)^2 Cycle 4, Chi^2= 1.00192 Current error model SIG(F2)^2 = 97.55*I_RAW + 3.87*I_BACK+(0.02458*)^2 Cycle 5, Chi^2= 1.00014 Current error model SIG(F2)^2 = 97.68*I_RAW + 3.86*I_BACK+(0.02472*)^2 Cycle 6, Chi^2= 1.00018 Current error model SIG(F2)^2 = 97.78*I_RAW + 3.84*I_BACK+(0.02468*)^2 Final Chi^2= 1.00018 Final error model SIG(F2)^2 = 97.78*I_RAW + 3.84*I_BACK+(0.02468*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1180812- 126797 206 377818.71 31.47 100.00 125804- 3676 206 29760.14 12.68 100.00 3662- 2036 206 2785.04 5.70 98.54 2031- 1221 206 1542.50 3.70 60.19 1218- 797 206 987.02 2.62 20.39 797- 533 206 668.63 2.23 10.68 532- 322 206 426.79 1.97 10.19 322- 141 206 227.18 1.36 2.91 141- 7 206 73.86 0.68 0.00 6- -1027 210 -140.30 -0.59 0.00 ------------------------------------------------------------------------------------ 1180812- -1027 2064 41334.42 6.17 40.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 206 97362.12 9.95 71.36 1.64- 1.26 206 76901.39 9.24 58.74 1.26- 1.06 206 65157.67 8.86 72.82 1.06- 0.97 206 41611.88 5.85 32.04 0.97- 0.88 206 23924.31 5.57 50.97 0.88- 0.80 206 41433.92 6.58 36.41 0.80- 0.75 206 20352.20 4.16 24.27 0.75- 0.71 206 21073.06 4.86 19.42 0.71- 0.67 206 22157.81 4.94 29.13 0.67- 0.63 210 4093.01 1.76 7.62 ------------------------------------------------------------------------------------ 6.00- 0.63 2064 41334.42 6.17 40.21 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 206 97362.12 9.95 71.36 6.00- 1.26 412 87131.76 9.59 65.05 6.00- 1.06 618 79807.06 9.35 67.64 6.00- 0.97 824 70258.27 8.47 58.74 6.00- 0.88 1030 60991.48 7.89 57.18 6.00- 0.80 1236 57731.88 7.67 53.72 6.00- 0.75 1442 52391.93 7.17 49.51 6.00- 0.71 1648 48477.07 6.88 45.75 6.00- 0.67 1854 45552.71 6.67 43.91 6.00- 0.63 2064 41334.42 6.17 40.21 ------------------------------------------------------------------------------------ 6.00- 0.63 2064 41334.42 6.17 40.21 Scale applied to data: s=0.846874 (maximum obs:1180812.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.070; Rsigma 0.037: data 2064 -> merged 162 With outlier rejection... Rint 0.057; Rsigma 0.037: data 2050 -> merged 162 Rejected total: 14, method kkm 13, method Blessing 1 Completeness direct cell (a, b, c) = (10.416, 10.416, 10.416), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626982, 6.013802 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.76 14 14 13.00 100.00 182 1.74 - 1.27 14 14 14.71 100.00 206 1.26 - 1.06 14 14 16.57 100.00 232 1.05 - 0.97 14 14 14.29 100.00 200 0.95 - 0.88 14 14 15.36 100.00 215 0.87 - 0.81 14 14 13.64 100.00 191 0.80 - 0.76 14 14 14.07 100.00 197 0.76 - 0.72 14 14 12.14 100.00 170 0.72 - 0.69 14 14 12.50 100.00 175 0.69 - 0.65 19 19 11.00 100.00 209 --------------------------------------------------------------- 7.37 - 0.65 145 145 13.63 100.00 1977 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:50:35 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.372270 7.367551 7.381422 120.2866 120.1130 89.6500 1970 Reflections read from file xs2212a.hkl 1970 Reflections used for space-group determination (up to diffraction limit of 0.46A); mean (I/sigma) = 4.50 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1001 993 988 992 1491 1308 1311 1970 N (int>3sigma) = 0 112 112 150 107 187 285 293 428 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 23.2 26.7 24.6 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.2 4.9 4.5 Lattice type: P chosen Volume: 282.65 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.343 7.364 7.368 119.96 119.76 90.09 Niggli form: a.a = 53.913 b.b = 54.232 c.c = 54.281 b.c = -27.095 a.c = -26.854 a.b = -0.089 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.406 CUBIC F-lattice R(int) = 0.209 [ 1734] Vol = 1130.6 Cell: 10.454 10.408 10.391 89.83 90.04 89.91 Volume: 1130.58 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.524 TETRAGONAL I-lattice R(int) = 0.162 [ 1385] Vol = 565.3 Cell: 7.370 7.381 10.391 90.09 89.85 89.74 Volume: 565.29 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.374 TETRAGONAL I-lattice R(int) = 0.195 [ 1381] Vol = 565.3 Cell: 7.343 7.364 10.454 90.03 89.91 90.09 Volume: 565.29 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.216 TETRAGONAL I-lattice R(int) = 0.162 [ 1385] Vol = 565.3 Cell: 7.381 7.370 10.391 90.15 90.09 90.26 Volume: 565.29 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.420 ORTHORHOMBIC F-lattice R(int) = 0.160 [ 1359] Vol = 1130.6 Cell: 10.391 10.408 10.454 89.91 90.04 89.83 Volume: 1130.58 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.543 ORTHORHOMBIC I-lattice R(int) = 0.124 [ 1334] Vol = 565.3 Cell: 10.391 7.381 7.370 89.74 89.85 90.09 Volume: 565.29 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.137 ORTHORHOMBIC I-lattice R(int) = 0.201 [ 1341] Vol = 565.3 Cell: 7.343 7.364 10.454 89.97 90.09 90.09 Volume: 565.29 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.349 MONOCLINIC I-lattice R(int) = 0.087 [ 938] Vol = 565.3 Cell: 7.370 10.391 7.381 90.09 90.26 90.15 Volume: 565.29 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.367 MONOCLINIC I-lattice R(int) = 0.155 [ 1016] Vol = 565.3 Cell: 7.368 10.408 7.372 89.94 90.35 89.82 Volume: 565.29 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.332 MONOCLINIC I-lattice R(int) = 0.087 [ 938] Vol = 565.3 Cell: 7.381 10.391 7.370 90.15 90.26 90.09 Volume: 565.29 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.091 MONOCLINIC I-lattice R(int) = 0.188 [ 1023] Vol = 565.3 Cell: 7.343 7.364 10.454 90.03 90.09 89.91 Volume: 565.29 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.062 MONOCLINIC I-lattice R(int) = 0.149 [ 921] Vol = 565.3 Cell: 7.343 10.454 7.364 90.03 90.09 89.91 Volume: 565.29 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.122 MONOCLINIC I-lattice R(int) = 0.149 [ 921] Vol = 565.3 Cell: 7.343 10.454 7.364 89.97 90.09 90.09 Volume: 565.29 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.077 [ 383] Vol = 282.6 Cell: 7.343 7.364 7.368 119.96 119.76 90.09 Volume: 282.65 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 0 988 0 1305 1314 1970 N (int>3sigma) = 0 0 0 0 150 0 297 300 428 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 25.3 24.7 24.6 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.5 4.6 4.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.815 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 12 12 151 368 N I>3s 0 0 1 90 0.1 0.1 -0.0 1.6 0.7 0.7 0.1 2.5 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 0.209 1611 Fd-3m 1 1 227 C N N N N 37 2284 0.209 1674 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.454413 10.407790 10.390745 89.8308 90.0367 89.9145 ZERR 1.00 0.001215 0.012944 0.006976 0.0002 0.0002 0.1340 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1099670- 102590 247 237 27 8.8 333754.97 29.80 0.051 0.058 78449- 1677 396 394 27 14.6 5640.48 7.83 0.129 0.178 1611- 875 395 394 27 14.6 1173.12 2.88 0.251 0.304 791- 370 367 367 27 13.6 550.25 2.02 0.368 0.463 368- 68 362 361 27 13.4 229.00 1.19 0.581 0.937 60- -337 297 297 27 11.0 -4.76 0.12 0.954 3.205 ------------------------------------------------------------------------------------------- 1099670- -337 2064 2050 162 12.7 40033.02 6.09 0.057 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-1.27 389 386 27 14.3 88284.63 9.96 0.053 0.055 0.028 1.26-0.97 436 432 28 15.4 48524.05 6.86 0.041 0.047 0.034 0.95-0.81 408 406 28 14.5 32987.62 6.13 0.067 0.086 0.043 0.80-0.73 358 356 27 13.2 18761.86 4.19 0.064 0.066 0.055 0.72-0.67 310 309 27 11.4 19809.07 4.46 0.079 0.099 0.062 0.66-0.63 163 161 25 6.4 5181.54 2.00 0.224 0.161 0.111 ------------------------------------------------------------------------------------------------------ inf-0.63 2064 2050 162 12.7 40033.02 6.09 0.057 0.063 0.037 inf-0.65 1987 1975 144 13.7 41209.02 6.23 0.055 0.061 0.037 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-1.27 386 27 27 100.0 14.3 88284.63 36.14 0.053 0.011 1.26-0.97 432 28 28 100.0 15.4 48524.05 25.64 0.041 0.011 0.95-0.81 406 28 28 100.0 14.5 32987.62 23.22 0.067 0.014 0.80-0.73 356 27 27 100.0 13.2 18761.86 14.15 0.064 0.019 0.72-0.67 309 27 27 100.0 11.4 19809.07 16.09 0.079 0.020 0.66-0.63 161 25 25 100.0 6.4 5181.54 5.24 0.224 0.048 -------------------------------------------------------------------------------------------- inf-0.63 2050 162 162 100.0 12.7 40033.02 22.10 0.057 0.013 inf-0.65 1975 144 144 100.0 13.7 41209.02 22.74 0.055 0.013 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 12:57:07 2019) ID: 3668; threads 40; handles 811; mem 515356.00 (1204688.00)kB; time: 1w 4d 23h 7m 55s MEMORY INFO: Memory PF:280.0, Ph:659.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.3,peak PF: 700.2, WS: 471.3, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:281.0, Ph:661.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.1,peak PF: 700.2, WS: 473.1, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 12:57:07 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000102 0.000064 0.000100 ) 0.064809 0.092374 0.027273 ( 0.000113 0.000071 0.000110 ) 0.045523 0.057900 0.132205 ( 0.000132 0.000083 0.000129 ) 7.38096 ( 0.00734 ) 7.36649 ( 0.00765 ) 7.42630 ( 0.00859 ) 120.52449 ( 0.11644 ) 120.40327 ( 0.11390 ) 89.27095 ( 0.08236 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.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 Wed Aug 21 12:57:07 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000102 0.000064 0.000100 ) 0.064809 0.092374 0.027273 ( 0.000113 0.000071 0.000110 ) 0.045523 0.057900 0.132205 ( 0.000132 0.000083 0.000129 ) M - matrix: 0.013828 0.004570 0.009203 ( 0.000026 0.000016 0.000022 ) 0.004570 0.013978 0.009342 ( 0.000016 0.000017 0.000018 ) 0.009203 0.009342 0.018474 ( 0.000022 0.000018 0.000035 ) unit cell: 7.381(7) 7.366(8) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 219 peaks identified as outliers and rejected 219 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 219 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 219 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.60 | 22 | 0.976 ( 0.491) | 0.868 ( 0.197) | 1.508 ( 2.006) | 2.57- 1.75 | 22 | 0.828 ( 0.083) | 0.818 ( 0.139) | 0.768 ( 0.416) | 1.75- 1.56 | 22 | 0.853 ( 0.097) | 0.888 ( 0.151) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.931 ( 0.058) | 0.996 ( 0.106) | 1.014 ( 0.487) | 1.35- 1.16 | 22 | 0.957 ( 0.073) | 1.048 ( 0.131) | 1.031 ( 0.679) | 1.16- 1.00 | 22 | 0.918 ( 0.088) | 0.925 ( 0.172) | 0.957 ( 0.410) | 1.00- 0.88 | 22 | 0.970 ( 0.073) | 1.007 ( 0.102) | 1.261 ( 0.532) | 0.88- 0.78 | 22 | 0.982 ( 0.054) | 1.024 ( 0.142) | 1.076 ( 0.312) | 0.78- 0.69 | 22 | 0.975 ( 0.044) | 0.942 ( 0.105) | 1.351 ( 0.495) | 0.69- 0.63 | 21 | 0.945 ( 0.035) | 0.924 ( 0.096) | 1.289 ( 0.448) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 219 | 0.933 ( 0.177) | 0.944 ( 0.155) | 1.092 ( 0.814) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 203 obs out of 219 (total:219,skipped:0) (92.69%) UB - matrix: 0.087419 -0.046181 0.017569 ( 0.000092 0.000059 0.000090 ) 0.064794 0.092241 0.027370 ( 0.000081 0.000052 0.000080 ) 0.045572 0.057566 0.131893 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013917 0.004563 0.009320 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009306 ( 0.000013 0.000014 0.000014 ) 0.009320 0.009306 0.018453 ( 0.000018 0.000014 0.000028 ) unit cell: 7.392(6) 7.371(6) 7.445(7) 120.44(9) 120.59(9) 89.15(7) V = 284.5(4) OTKP changes: 204 1 1 1 OTKP changes: 204 1 1 1 OTKP changes: 204 1 1 1 UB - matrix: 0.087484 -0.046073 0.017374 ( 0.000096 0.000062 0.000093 ) 0.064688 0.092374 0.027176 ( 0.000085 0.000055 0.000082 ) 0.045724 0.057888 0.132160 ( 0.000099 0.000064 0.000096 ) M - matrix: 0.013929 0.004592 0.009321 ( 0.000022 0.000013 0.000017 ) 0.004592 0.014007 0.009360 ( 0.000013 0.000014 0.000014 ) 0.009321 0.009360 0.018507 ( 0.000017 0.000014 0.000026 ) UB fit with 208 obs out of 219 (total:219,skipped:0) (94.98%) unit cell: 7.382(6) 7.367(6) 7.434(6) 120.52(9) 120.45(9) 89.24(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087484 -0.046073 0.017374 ( 0.000096 0.000062 0.000093 ) 0.064688 0.092374 0.027175 ( 0.000085 0.000055 0.000082 ) 0.045724 0.057888 0.132160 ( 0.000099 0.000064 0.000096 ) M - matrix: 0.013929 0.004592 0.009321 ( 0.000022 0.000013 0.000017 ) 0.004592 0.014007 0.009360 ( 0.000013 0.000014 0.000014 ) 0.009321 0.009360 0.018507 ( 0.000017 0.000014 0.000026 ) UB fit with 208 obs out of 219 (total:219,skipped:0) (94.98%) unit cell: 7.382(6) 7.367(6) 7.434(6) 120.52(9) 120.45(9) 89.24(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 213 obs out of 219 (total:219,skipped:0) (97.26%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.781 ( 0.325) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.931 ( 0.073) | 0.994 ( 0.133) | 1.105 ( 0.542) | 1.35- 1.16 | 21 | 0.967 ( 0.064) | 1.042 ( 0.104) | 0.943 ( 0.383) | 1.16- 1.00 | 21 | 0.933 ( 0.077) | 0.960 ( 0.178) | 0.943 ( 0.411) | 1.00- 0.88 | 21 | 0.970 ( 0.076) | 1.010 ( 0.131) | 1.205 ( 0.518) | 0.88- 0.79 | 21 | 0.978 ( 0.051) | 1.013 ( 0.138) | 1.189 ( 0.365) | 0.79- 0.72 | 21 | 0.980 ( 0.042) | 0.953 ( 0.119) | 1.255 ( 0.471) | 0.69- 0.63 | 23 | 0.954 ( 0.039) | 0.934 ( 0.099) | 1.324 ( 0.488) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.939 ( 0.191) | 0.946 ( 0.157) | 1.106 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.934 ( 0.070) | 0.935 ( 0.100) | 1.000 ( 0.370) | 0.82- 0.73 | 25 | 0.950 ( 0.054) | 0.897 ( 0.086) | 1.416 ( 0.422) | 0.72- 0.63 | 27 | 0.932 ( 0.035) | 0.887 ( 0.094) | 1.339 ( 0.472) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 252 | 0.920 ( 0.080) | 0.918 ( 0.122) | 1.053 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014043 ( 0.000043 0.000052 0.000055 ) 0.061983 0.093199 0.025299 ( 0.000038 0.000046 0.000049 ) 0.048732 0.057069 0.133852 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018754 ( 0.000008 0.000009 0.000015 ) unit cell: 7.378(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.71(4) V = 280.9(2) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 UB - matrix: 0.087515 -0.045162 0.014031 ( 0.000046 0.000056 0.000059 ) 0.062005 0.093008 0.025382 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057046 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013944 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009280 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014031 ( 0.000046 0.000056 0.000059 ) 0.062005 0.093008 0.025382 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057046 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013944 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009280 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.879 ( 0.098) | 0.890 ( 0.140) | 0.977 ( 0.519) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.984 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | 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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb PROFFITPEAK info: 130 peaks in the peak location table UB fit with 23 obs out of 64 (total:64,skipped:0) (35.94%) UB - matrix: 0.087156 -0.045109 0.014542 ( 0.000219 0.000389 0.000737 ) 0.064707 0.092250 0.028198 ( 0.000188 0.000335 0.000634 ) 0.045562 0.058346 0.131822 ( 0.000181 0.000322 0.000610 ) M - matrix: 0.013859 0.004696 0.009098 ( 0.000048 0.000048 0.000085 ) 0.004696 0.013949 0.009637 ( 0.000048 0.000080 0.000088 ) 0.009098 0.009637 0.018384 ( 0.000085 0.000088 0.000166 ) unit cell: 7.33(3) 7.52(3) 7.50(4) 122.0(5) 119.2(5) 89.5(3) V = 288(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 23 obs out of 64 (total:64,skipped:0) (35.94%) UB - matrix: 0.087156 -0.045109 0.014542 ( 0.000219 0.000389 0.000737 ) 0.064707 0.092250 0.028198 ( 0.000188 0.000335 0.000634 ) 0.045562 0.058346 0.131822 ( 0.000181 0.000322 0.000610 ) M - matrix: 0.013859 0.004696 0.009098 ( 0.000048 0.000048 0.000085 ) 0.004696 0.013949 0.009637 ( 0.000048 0.000080 0.000088 ) 0.009098 0.009637 0.018384 ( 0.000085 0.000088 0.000166 ) unit cell: 7.33(3) 7.52(3) 7.50(4) 122.0(5) 119.2(5) 89.5(3) V = 288(2) OTKP changes: 15 1 1 1 OTKP changes: 15 1 1 1 OTKP changes: 15 1 1 1 UB - matrix: 0.088004 -0.044393 0.013538 ( 0.000050 0.000061 0.000112 ) 0.061716 0.093991 0.025835 ( 0.000083 0.000102 0.000186 ) 0.048614 0.056135 0.132974 ( 0.000100 0.000123 0.000224 ) M - matrix: 0.013917 0.004623 0.009250 ( 0.000017 0.000014 0.000023 ) 0.004623 0.013956 0.009292 ( 0.000014 0.000024 0.000028 ) 0.009250 0.009292 0.018533 ( 0.000023 0.000028 0.000060 ) UB fit with 61 obs out of 64 (total:64,skipped:0) (95.31%) unit cell: 7.355(6) 7.356(9) 7.367(13) 120.09(16) 119.94(13) 89.91(8) V = 281.9(7) UB fit with 61 obs out of 64 (total:64,skipped:0) (95.31%) UB - matrix: 0.088004 -0.044393 0.013538 ( 0.000050 0.000061 0.000112 ) 0.061717 0.093991 0.025835 ( 0.000083 0.000102 0.000186 ) 0.048614 0.056135 0.132974 ( 0.000100 0.000123 0.000224 ) M - matrix: 0.013917 0.004623 0.009250 ( 0.000017 0.000014 0.000023 ) 0.004623 0.013956 0.009292 ( 0.000014 0.000024 0.000028 ) 0.009250 0.009292 0.018533 ( 0.000023 0.000028 0.000060 ) unit cell: 7.355(6) 7.356(9) 7.367(13) 120.09(16) 119.94(13) 89.91(8) V = 281.9(7) OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 UB - matrix: 0.088042 -0.044395 0.013540 ( 0.000049 0.000061 0.000111 ) 0.061712 0.094005 0.025837 ( 0.000083 0.000102 0.000186 ) 0.048592 0.056119 0.132950 ( 0.000100 0.000122 0.000223 ) M - matrix: 0.013921 0.004619 0.009247 ( 0.000017 0.000014 0.000023 ) 0.004619 0.013957 0.009289 ( 0.000014 0.000024 0.000028 ) 0.009247 0.009289 0.018527 ( 0.000023 0.000028 0.000060 ) UB fit with 61 obs out of 64 (total:64,skipped:0) (95.31%) unit cell: 7.353(6) 7.355(9) 7.367(13) 120.10(16) 119.94(13) 89.90(8) V = 281.8(7) 64 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Run 3 Omega scan: (-48.000 - -23.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 459 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 61 obs out of 64 (total:64,skipped:0) (95.31%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb 0 of 53 peaks identified as outliers and rejected 53 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 53 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 53 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.12- 2.35 | 5 | 0.855 ( 0.082) | 0.872 ( 0.112) | 1.154 ( 0.420) | 2.11- 1.76 | 5 | 0.855 ( 0.125) | 0.833 ( 0.152) | 0.661 ( 0.221) | 1.75- 1.58 | 5 | 0.921 ( 0.061) | 0.940 ( 0.119) | 0.839 ( 0.113) | 1.57- 1.45 | 5 | 0.931 ( 0.099) | 0.952 ( 0.135) | 0.750 ( 0.117) | 1.36- 1.22 | 5 | 0.935 ( 0.081) | 0.899 ( 0.168) | 0.911 ( 0.511) | 1.20- 1.16 | 5 | 0.947 ( 0.098) | 0.930 ( 0.169) | 0.757 ( 0.181) | 1.10- 0.92 | 5 | 0.962 ( 0.085) | 0.943 ( 0.127) | 0.920 ( 0.440) | 0.88- 0.82 | 5 | 1.005 ( 0.042) | 0.955 ( 0.055) | 0.902 ( 0.335) | 0.79- 0.72 | 5 | 0.967 ( 0.048) | 0.943 ( 0.136) | 1.362 ( 0.607) | 0.69- 0.63 | 8 | 0.945 ( 0.062) | 0.828 ( 0.081) | 0.912 ( 0.132) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.12- 0.63 | 53 | 0.933 ( 0.092) | 0.905 ( 0.137) | 0.917 ( 0.392) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 53 obs out of 53 (total:53,skipped:0) (100.00%) UB - matrix: 0.088223 -0.044393 0.013516 ( 0.000065 0.000072 0.000146 ) 0.061799 0.094081 0.026022 ( 0.000042 0.000047 0.000095 ) 0.048575 0.055853 0.132909 ( 0.000065 0.000072 0.000146 ) M - matrix: 0.013962 0.004611 0.009257 ( 0.000014 0.000010 0.000018 ) 0.004611 0.013942 0.009272 ( 0.000010 0.000014 0.000017 ) 0.009257 0.009272 0.018525 ( 0.000018 0.000017 0.000039 ) unit cell: 7.341(6) 7.355(6) 7.364(8) 120.07(10) 119.95(10) 89.86(6) V = 281.4(5) OTKP changes: 53 1 1 1 OTKP changes: 53 1 1 1 OTKP changes: 53 1 1 1 UB - matrix: 0.087998 -0.044404 0.013563 ( 0.000037 0.000041 0.000082 ) 0.061848 0.094000 0.025994 ( 0.000043 0.000047 0.000095 ) 0.048745 0.056018 0.133059 ( 0.000048 0.000053 0.000106 ) M - matrix: 0.013945 0.004637 0.009287 ( 0.000010 0.000007 0.000012 ) 0.004637 0.013946 0.009295 ( 0.000007 0.000011 0.000013 ) 0.009287 0.009295 0.018564 ( 0.000012 0.000013 0.000029 ) UB fit with 53 obs out of 53 (total:53,skipped:0) (100.00%) unit cell: 7.356(4) 7.358(5) 7.366(6) 120.06(8) 120.02(7) 89.92(5) V = 281.8(3) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - -23.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 462 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 53 obs out of 53 (total:53,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb 0 of 54 peaks identified as outliers and rejected 54 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 54 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 54 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.58 | 5 | 0.820 ( 0.090) | 0.797 ( 0.108) | 1.086 ( 0.458) | 2.38- 1.99 | 5 | 0.858 ( 0.095) | 0.871 ( 0.122) | 0.708 ( 0.203) | 1.83- 1.75 | 5 | 0.934 ( 0.089) | 0.946 ( 0.137) | 0.782 ( 0.172) | 1.65- 1.46 | 5 | 0.936 ( 0.099) | 0.969 ( 0.135) | 0.823 ( 0.128) | 1.45- 1.35 | 5 | 0.920 ( 0.083) | 0.891 ( 0.173) | 0.750 ( 0.165) | 1.22- 1.16 | 5 | 0.957 ( 0.094) | 0.916 ( 0.174) | 1.027 ( 0.423) | 1.16- 0.92 | 5 | 0.964 ( 0.085) | 0.940 ( 0.128) | 0.928 ( 0.431) | 0.92- 0.87 | 5 | 1.001 ( 0.048) | 0.967 ( 0.043) | 0.885 ( 0.355) | 0.82- 0.73 | 5 | 0.969 ( 0.048) | 0.956 ( 0.128) | 0.991 ( 0.384) | 0.72- 0.63 | 9 | 0.945 ( 0.057) | 0.835 ( 0.082) | 1.074 ( 0.486) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 54 | 0.931 ( 0.094) | 0.903 ( 0.138) | 0.918 ( 0.382) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-11.1 | 52 | 0.973 ( 0.040) | 1.006 ( 0.085) | 1.138 ( 0.444) | 11.3-15.1 | 52 | 0.982 ( 0.045) | 1.044 ( 0.072) | 1.148 ( 0.520) | 15.1-19.7 | 52 | 0.994 ( 0.288) | 1.011 ( 0.111) | 1.254 ( 1.461) | 19.7-23.9 | 52 | 0.954 ( 0.051) | 0.998 ( 0.078) | 0.941 ( 0.400) | 24.0-27.5 | 52 | 0.954 ( 0.072) | 0.993 ( 0.105) | 0.975 ( 0.447) | 27.6-33.4 | 52 | 0.919 ( 0.076) | 0.931 ( 0.109) | 0.929 ( 0.453) | 33.4-36.8 | 52 | 0.918 ( 0.200) | 0.884 ( 0.127) | 1.135 ( 0.762) | 36.8-39.1 | 52 | 0.862 ( 0.084) | 0.829 ( 0.110) | 0.999 ( 0.497) | 39.1-42.0 | 52 | 0.889 ( 0.094) | 0.828 ( 0.122) | 1.102 ( 0.493) | 42.0-50.1 | 52 | 0.865 ( 0.105) | 0.775 ( 0.117) | 0.981 ( 0.487) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 520 | 0.931 ( 0.137) | 0.930 ( 0.138) | 1.060 ( 0.677) | Fitted profile normalization line parameters e1 dimension: a=-0.0038 b=1.15 e2 dimension: a=-0.0080 b=1.28 e3 dimension: a=0.0035 b=0.98 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336998 PROFFITPEAK - Finished at Wed Aug 21 12:57:16 2019 PROFFITMAIN - Started at Wed Aug 21 12:57:16 2019 OTKP changes: 276 2 2 3 OTKP changes: 276 2 2 3 OTKP changes: 276 2 2 3 UB - matrix: 0.087595 -0.046081 0.017005 ( 0.000092 0.000061 0.000092 ) 0.063919 0.092453 0.027114 ( 0.000104 0.000068 0.000103 ) 0.045507 0.057687 0.132173 ( 0.000113 0.000074 0.000112 ) M - matrix: 0.013829 0.004498 0.009237 ( 0.000023 0.000015 0.000019 ) 0.004498 0.013999 0.009348 ( 0.000015 0.000016 0.000016 ) 0.009237 0.009348 0.018494 ( 0.000019 0.000016 0.000030 ) UB fit with 301 obs out of 520 (total:520,skipped:0) (57.88%) unit cell: 7.390(7) 7.367(7) 7.430(8) 120.69(11) 120.40(10) 88.94(8) V = 283.9(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) UB - matrix: 0.087507 -0.046193 0.017357 ( 0.000099 0.000062 0.000094 ) 0.064805 0.092368 0.027249 ( 0.000087 0.000054 0.000082 ) 0.045929 0.057757 0.132142 ( 0.000106 0.000066 0.000100 ) M - matrix: 0.013967 0.004596 0.009354 ( 0.000023 0.000013 0.000018 ) 0.004596 0.014002 0.009347 ( 0.000013 0.000014 0.000014 ) 0.009354 0.009347 0.018505 ( 0.000018 0.000014 0.000027 ) unit cell: 7.380(6) 7.364(6) 7.438(7) 120.47(9) 120.56(9) 89.21(7) V = 283.3(4) OTKP changes: 201 1 1 1 OTKP changes: 201 1 1 1 OTKP changes: 201 1 1 1 UB - matrix: 0.087340 -0.045981 0.017444 ( 0.000097 0.000060 0.000092 ) 0.064681 0.092309 0.027283 ( 0.000086 0.000053 0.000081 ) 0.045519 0.057795 0.131989 ( 0.000103 0.000064 0.000097 ) M - matrix: 0.013884 0.004585 0.009296 ( 0.000022 0.000013 0.000017 ) 0.004585 0.013975 0.009345 ( 0.000013 0.000014 0.000013 ) 0.009296 0.009345 0.018470 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.394(6) 7.377(6) 7.441(6) 120.53(9) 120.43(9) 89.27(7) V = 284.6(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.105) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087340 -0.045981 0.017444 ( 0.000097 0.000060 0.000092 ) 0.064681 0.092309 0.027284 ( 0.000086 0.000053 0.000081 ) 0.045517 0.057795 0.131989 ( 0.000103 0.000064 0.000097 ) M - matrix: 0.013884 0.004585 0.009296 ( 0.000022 0.000013 0.000017 ) 0.004585 0.013975 0.009345 ( 0.000013 0.000014 0.000013 ) 0.009296 0.009345 0.018470 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.394(6) 7.377(6) 7.441(6) 120.53(9) 120.43(9) 89.27(7) V = 284.6(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118025 0.039097 0.078751 ( 0.000075 0.000047 0.000069 ) 0.000038 0.111522 0.056228 ( 0.000075 0.000047 0.000069 ) 0.000031 -0.000042 0.095480 ( 0.000091 0.000057 0.000084 ) M - matrix: 0.013930 0.004619 0.009300 ( 0.000018 0.000010 0.000014 ) 0.004619 0.013966 0.009346 ( 0.000010 0.000011 0.000011 ) 0.009300 0.009346 0.018480 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.375(5) 7.379(5) 7.428(8) 120.46(9) 120.28(9) 89.48(5) V = 284.0(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009290 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009290 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 54 obs out of 54 (total:54,skipped:0) (100.00%) UB - matrix: 0.087994 -0.044392 0.013546 ( 0.000035 0.000040 0.000079 ) 0.061841 0.094019 0.025963 ( 0.000041 0.000046 0.000092 ) 0.048743 0.056011 0.133061 ( 0.000049 0.000055 0.000108 ) M - matrix: 0.013943 0.004638 0.009283 ( 0.000009 0.000007 0.000012 ) 0.004638 0.013948 0.009293 ( 0.000007 0.000011 0.000013 ) 0.009283 0.009293 0.018563 ( 0.000012 0.000013 0.000029 ) unit cell: 7.355(4) 7.357(4) 7.364(6) 120.04(8) 120.00(7) 89.94(4) V = 281.7(3) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087931 -0.044372 0.013554 ( 0.000036 0.000040 0.000079 ) 0.061842 0.093948 0.025995 ( 0.000041 0.000046 0.000091 ) 0.048677 0.055985 0.132934 ( 0.000048 0.000054 0.000107 ) M - matrix: 0.013926 0.004633 0.009270 ( 0.000009 0.000007 0.000012 ) 0.004633 0.013929 0.009283 ( 0.000007 0.000011 0.000013 ) 0.009270 0.009283 0.018531 ( 0.000012 0.000013 0.000029 ) UB fit with 54 obs out of 54 (total:54,skipped:0) (100.00%) unit cell: 7.360(4) 7.363(4) 7.372(6) 120.06(8) 120.00(7) 89.93(4) V = 282.4(3) Run 3 Omega scan: (-48.000 - -23.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.056) HKL list info: 436 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* UB - matrix: 0.087931 -0.044372 0.013554 ( 0.000036 0.000040 0.000079 ) 0.061842 0.093948 0.025995 ( 0.000041 0.000046 0.000091 ) 0.048677 0.055985 0.132934 ( 0.000048 0.000054 0.000107 ) M - matrix: 0.013926 0.004633 0.009270 ( 0.000009 0.000007 0.000012 ) 0.004633 0.013929 0.009283 ( 0.000007 0.000011 0.000013 ) 0.009270 0.009283 0.018531 ( 0.000012 0.000013 0.000029 ) UB fit with 54 obs out of 54 (total:54,skipped:0) (100.00%) unit cell: 7.360(4) 7.363(4) 7.372(6) 120.06(8) 120.00(7) 89.93(4) V = 282.4(3) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117901 0.039080 0.078711 ( 0.000033 0.000031 0.000038 ) 0.000033 0.111495 0.056231 ( 0.000032 0.000031 0.000037 ) -0.000015 -0.000134 0.096015 ( 0.000040 0.000038 0.000046 ) M - matrix: 0.013901 0.004611 0.009281 ( 0.000008 0.000005 0.000007 ) 0.004611 0.013958 0.009333 ( 0.000005 0.000007 0.000006 ) 0.009281 0.009333 0.018576 ( 0.000007 0.000006 0.000011 ) UB fit with 515 obs out of 520 (total:520,skipped:0) (99.04%) unit cell: 7.369(3) 7.367(3) 7.382(4) 120.28(5) 120.10(5) 89.68(3) V = 282.5(2) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 69 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof 2301 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 12:57:20 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.105) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - -23.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.056) PROFFIT INFO: signal sum: min=-580.0000 max=7903371.0000 PROFFIT INFO: signal sum lp corr: min=-607.3175 max=1115342.2273 PROFFIT INFO: background sum: min=116.0000 max=7453.0000 PROFFIT INFO: background sum sig2: min=348.0000 max=4924.0000 PROFFIT INFO: num of signal pixels: min=29 max=490 PROFFIT INFO: Inet: min=-971.7080 max=1784547.6250 PROFFIT INFO: sig(Inet): min=64.2045 max=24341.2070 PROFFIT INFO: Inet/sig(Inet): min=-1.66 max=199.93 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 212 802 1199 1440 1549 1791 1939 2033 2180 2277 2301 Percent 9.2 34.9 52.1 62.6 67.3 77.8 84.3 88.4 94.7 99.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2301 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 2301 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1784548- 127694 230 397759.14 75.88 100.00 127308- 4034 230 28660.15 19.80 100.00 3996- 2051 230 2862.69 7.16 97.83 2050- 1232 230 1588.56 3.86 52.17 1231- 812 230 1001.92 2.13 9.57 811- 541 230 665.98 1.64 6.52 540- 322 230 430.91 1.30 7.39 321- 146 230 228.00 0.66 0.87 146- 8 230 72.38 0.26 0.00 8- -972 231 -141.66 -0.27 0.00 ------------------------------------------------------------------------------------ 1784548- -972 2301 43293.92 11.24 37.42 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.64 230 99244.66 16.53 69.13 1.64- 1.26 230 89860.02 20.81 58.26 1.26- 1.06 230 47453.09 13.56 48.70 1.06- 0.93 230 33289.12 10.81 41.74 0.93- 0.84 230 45467.34 12.88 32.17 0.84- 0.76 230 29673.99 9.60 33.91 0.76- 0.70 230 34501.40 10.24 31.74 0.70- 0.65 230 14984.95 5.30 18.70 0.65- 0.59 230 24312.47 7.82 24.78 0.59- 0.46 231 14278.32 4.85 15.15 ------------------------------------------------------------------------------------ 6.55- 0.46 2301 43293.92 11.24 37.42 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:57:20 2019 Sorting 2301 observations 71 unique observations with > 7.00 F2/sig(F2) 2301 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 24 230 Total number of frames 230 Maximum number of 71 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 2301 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 6 59 Total number of frames 59 555 observations > 7.00 F2/sig(F2) 555 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 5 58 Total number of frames 58 Removing 'redundancy=1' reflections Average redundancy: 5.2 (Out of 555 removed 46 = 509, unique = 97) 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 509 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 5 58 Total number of frames 58 97 unique data precomputed (should be 97) 97 unique data with 509 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.2 (Out of 509 removed 0 = 509, unique = 97) 97 unique data precomputed (should be 97) 97 unique data with 509 observations RMS deviation of equivalent data = 0.38362 Rint = 0.35067 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.35067, wR= 0.47666 Trying model 1 (ne=2, no=0)... Results: Rint= 0.24581, wR= 0.33404, Acormin=0.463, Acormax=1.598, Acor_av=0.952 F test: Probability=1.000, F= 2.010 Trying model 2 (ne=2, no=1)... Results: Rint= 0.24441, wR= 0.33716, Acormin=0.216, Acormax=1.781, Acor_av=0.844 F test: Probability=0.516, F= 1.004 Trying model 3 (ne=4, no=0)... Results: Rint= 0.24735, wR= 0.30414, Acormin=0.237, Acormax=2.124, Acor_av=0.805 F test: Probability=0.000, F= 0.966 Trying model 4 (ne=4, no=1)... Results: Rint= 0.24465, wR= 0.30603, Acormin=0.110, Acormax=2.037, Acor_av=0.766 F test: Probability=0.000, F= 0.980 Trying model 5 (ne=4, no=3)... Results: Rint= 0.24869, wR= 0.28796, Acormin=0.132, Acormax=1.875, Acor_av=0.637 F test: Probability=0.000, F= 0.931 Trying model 6 (ne=6, no=0)... Results: Rint= 0.24361, wR= 0.29750, Acormin=0.206, Acormax=2.306, Acor_av=0.772 F test: Probability=0.000, F= 0.963 Trying model 7 (ne=6, no=1)... Results: Rint= 0.24526, wR= 0.29720, Acormin=0.030, Acormax=2.337, Acor_av=0.741 F test: Probability=0.000, F= 0.943 Trying model 8 (ne=6, no=3)... Results: Rint= 0.24071, wR= 0.27377, Acormin=0.067, Acormax=1.976, Acor_av=0.609 F test: Probability=0.000, F= 0.961 Trying model 9 (ne=6, no=5)... Results: Rint= 0.24675, wR= 0.27439, Acormin=-0.168, Acormax=1.300, Acor_av=0.389 F test: Probability=0.000, F= 0.888 Trying model 10 (ne=8, no=0)... Results: Rint= 0.24813, wR= 0.29538, Acormin=0.073, Acormax=2.276, Acor_av=0.679 F test: Probability=0.000, F= 0.887 Trying model 11 (ne=8, no=1)... Results: Rint= 0.32427, wR= 0.37107, Acormin=-0.178, Acormax=1.694, Acor_av=0.435 F test: Probability=0.000, F= 0.515 Trying model 12 (ne=8, no=3)... Results: Rint= 0.24505, wR= 0.26841, Acormin=-0.007, Acormax=0.162, Acor_av=0.051 F test: Probability=0.000, F= 0.885 Trying model 13 (ne=8, no=5)... Results: Rint= 0.20175, wR= 0.22062, Acormin=-0.001, Acormax=0.184, Acor_av=0.062 F test: Probability=0.988, F= 1.266 Trying model 14 (ne=8, no=7)... Results: Rint= 0.13637, wR= 0.17954, Acormin=0.012, Acormax=0.235, Acor_av=0.072 F test: Probability=1.000, F= 2.651 Final absorption model (ne=2, no=0): Rint= 0.24581, Acormin=0.463, Acormax=1.598, Acor_av=0.952 Combined refinement in use Rint: 0.36563 There are 58 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 62 pars with 1953 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.38362 Using Levenberg-Marquardt: 0.00010 New wR= 0.21558 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35067 with corrections 0.18174 Rint for all data: 0.36563 with corrections 0.19873 0 observations identified as outliers and rejected Cycle 2 wR= 0.21558 Using Levenberg-Marquardt: 0.00001 New wR= 0.20858 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35067 with corrections 0.17566 Rint for all data: 0.36563 with corrections 0.19280 0 observations identified as outliers and rejected Cycle 3 wR= 0.20858 Using Levenberg-Marquardt: 0.00000 New wR= 0.29794 Using Levenberg-Marquardt: 0.00001 New wR= 0.29753 Using Levenberg-Marquardt: 0.00010 New wR= 0.29355 Using Levenberg-Marquardt: 0.00100 New wR= 0.26285 Using Levenberg-Marquardt: 0.01000 New wR= 0.20441 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35067 with corrections 0.16786 Rint for all data: 0.36563 with corrections 0.18527 0 observations identified as outliers and rejected Cycle 4 wR= 0.20441 Using Levenberg-Marquardt: 0.00100 New wR= 0.20406 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35067 with corrections 0.17121 Rint for all data: 0.36563 with corrections 0.18837 0 observations identified as outliers and rejected Cycle 5 wR= 0.20406 Using Levenberg-Marquardt: 0.00010 New wR= 0.24288 Using Levenberg-Marquardt: 0.00100 New wR= 0.22788 Using Levenberg-Marquardt: 0.01000 New wR= 0.20067 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35067 with corrections 0.16743 Rint for all data: 0.36563 with corrections 0.18479 0 observations identified as outliers and rejected Final wR= 0.20067 Final frame scales: Min= 0.4382 Max= 1.5139 Final absorption correction factors: Amin= 0.3649 Amax= 1.5449 PROFFIT INFO: Inet (after scale3 abspack): min=-1717.8636 max=1484698.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=40.6033 max=25046.9980 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/103 2301 reflections read from tmp file 621 reflections are rejected (544 as outliers, 77 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 53 61 43 35 28 36 20 11 32 Initial Chi^2= 2.66309 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.81768 Current error model SIG(F2)^2 = 593.03*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 484.91*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 484.91*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1484699- 112049 230 359352.80 29.47 100.00 111201- 4029 230 25757.33 6.33 79.13 3997- 1925 230 2670.09 2.50 23.04 1914- 1154 230 1495.58 1.82 12.17 1151- 735 230 928.48 1.27 1.74 731- 482 230 607.39 1.04 0.43 481- 293 230 380.39 0.96 0.43 292- 133 230 211.51 0.76 0.43 132- 8 230 65.77 0.42 0.00 8- -1718 231 -167.35 -0.32 0.00 ------------------------------------------------------------------------------------ 1484699- -1718 2301 39113.12 4.42 21.73 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.64 230 94823.04 9.94 47.83 1.64- 1.26 230 85100.83 8.24 38.26 1.26- 1.06 230 41093.43 5.31 29.57 1.06- 0.93 230 38104.60 3.64 14.78 0.93- 0.84 230 37135.02 4.19 17.39 0.84- 0.76 230 28427.97 3.22 15.65 0.76- 0.70 230 27951.46 3.38 18.70 0.70- 0.65 230 10205.67 1.92 6.52 0.65- 0.59 230 19352.33 2.68 17.83 0.59- 0.46 231 9067.50 1.72 10.82 ------------------------------------------------------------------------------------ 6.55- 0.46 2301 39113.12 4.42 21.73 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.64 230 94823.04 9.94 47.83 6.55- 1.26 460 89961.93 9.09 43.04 6.55- 1.06 690 73672.43 7.83 38.55 6.55- 0.93 920 64780.47 6.78 32.61 6.55- 0.84 1150 59251.38 6.26 29.57 6.55- 0.76 1380 54114.15 5.76 27.25 6.55- 0.70 1610 50376.62 5.42 26.02 6.55- 0.65 1840 45355.25 4.98 23.59 6.55- 0.59 2070 42466.04 4.72 22.95 6.55- 0.46 2301 39113.12 4.42 21.73 ------------------------------------------------------------------------------------ 6.55- 0.46 2301 39113.12 4.42 21.73 Scale applied to data: s=0.673537 (maximum obs:1484698.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.185; Rsigma 0.055: data 2301 -> merged 402 With outlier rejection... Rint 0.166; Rsigma 0.055: data 2224 -> merged 402 Rejected total: 77, method kkm 70, method Blessing 7 Completeness direct cell (a, b, c) = (6.562, 6.562, 6.562), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.457187, 6.561861 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.59 22 22 11.59 100.00 255 1.55 - 1.22 22 22 11.27 100.00 248 1.20 - 1.02 22 22 10.00 100.00 220 1.02 - 0.92 22 22 8.73 100.00 192 0.92 - 0.84 22 22 8.45 100.00 186 0.84 - 0.79 22 22 6.73 100.00 148 0.79 - 0.75 22 22 6.82 100.00 150 0.75 - 0.71 22 22 5.73 100.00 126 0.71 - 0.69 22 22 5.73 100.00 126 0.68 - 0.65 26 29 5.08 89.66 132 --------------------------------------------------------------- 7.37 - 0.65 224 227 7.96 98.68 1783 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:57:21 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.369438 7.367192 7.381632 120.2763 120.1020 89.6834 2224 Reflections read from file xs2212a.hkl 2145 Reflections used for space-group determination (up to diffraction limit of 0.65A); mean (I/sigma) = 4.41 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1084 1070 1078 1077 1616 1414 1419 2145 N (int>3sigma) = 0 110 109 153 101 186 299 305 455 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 24.7 27.7 25.9 Mean int/sigma = 0.0 1.3 1.3 1.8 1.3 1.5 4.2 4.7 4.4 Lattice type: P chosen Volume: 282.54 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 1.0000 Unitcell: 7.344 7.364 7.367 60.01 60.13 89.91 Niggli form: a.a = 53.929 b.b = 54.231 c.c = 54.271 b.c = 27.113 a.c = 26.945 a.b = 0.088 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.536 CUBIC F-lattice R(int) = 0.220 [ 1935] Vol = 1130.2 Cell: 10.408 10.392 10.449 90.02 90.11 90.16 Volume: 1130.16 Matrix:-1.0000 -1.0000 -2.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.526 TETRAGONAL I-lattice R(int) = 0.170 [ 1586] Vol = 565.1 Cell: 7.367 7.369 10.408 90.03 89.81 89.68 Volume: 565.08 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.349 TETRAGONAL I-lattice R(int) = 0.204 [ 1602] Vol = 565.1 Cell: 7.344 7.364 10.449 89.93 89.91 89.91 Volume: 565.08 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.330 ORTHORHOMBIC F-lattice R(int) = 0.170 [ 1577] Vol = 1130.2 Cell: 10.408 10.392 10.449 89.98 90.11 89.84 Volume: 1130.16 Matrix: 1.0000 1.0000 2.0000 1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.532 ORTHORHOMBIC I-lattice R(int) = 0.177 [ 1522] Vol = 565.1 Cell: 10.408 7.369 7.367 89.68 89.81 90.03 Volume: 565.08 Matrix: 1.0000 1.0000 2.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.090 ORTHORHOMBIC I-lattice R(int) = 0.203 [ 1548] Vol = 565.1 Cell: 7.344 7.364 10.449 90.07 90.09 89.91 Volume: 565.08 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.325 MONOCLINIC I-lattice R(int) = 0.102 [ 1164] Vol = 565.1 Cell: 7.367 10.392 7.382 90.10 90.22 90.13 Volume: 565.08 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.314 MONOCLINIC I-lattice R(int) = 0.167 [ 1155] Vol = 565.1 Cell: 7.369 10.408 7.367 90.19 90.32 90.03 Volume: 565.08 Matrix:-1.0000 0.0000 0.0000 1.0000 1.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.090 MONOCLINIC I-lattice R(int) = 0.160 [ 1097] Vol = 565.1 Cell: 7.364 7.344 10.449 89.91 90.07 90.09 Volume: 565.08 Matrix: 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.088 MONOCLINIC I-lattice R(int) = 0.201 [ 1182] Vol = 565.1 Cell: 7.344 7.364 10.449 89.93 90.09 90.09 Volume: 565.08 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.096 [ 495] Vol = 282.5 Cell: 7.344 7.364 7.367 60.01 60.13 89.91 Volume: 282.54 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 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 1078 0 1414 1416 2145 N (int>3sigma) = 0 0 0 0 153 0 299 316 455 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 24.7 26.8 25.9 Mean int/sigma = 0.0 0.0 0.0 0.0 1.8 0.0 4.2 4.4 4.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.125 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 11 11 157 403 N I>3s 0 0 0 88 0.1 0.1 0.0 1.6 0.6 0.6 0.2 2.4 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 0.220 1802 Fd-3m 1 1 227 C N N N N 37 2284 0.220 1859 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.408403 10.391541 10.449121 90.0175 90.1146 90.1602 ZERR 1.00 0.011870 0.006367 0.001112 0.0006 0.1236 0.0005 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 940403- 110403 246 230 40 5.8 339608.93 28.34 0.148 0.147 97946- 2730 247 231 40 5.8 14824.53 4.47 0.294 0.159 2699- 1561 400 386 40 9.7 2056.96 2.06 0.818 0.928 1554- 1038 310 302 40 7.5 1160.05 1.28 0.738 0.796 1033- 808 250 241 40 6.0 781.64 1.01 0.707 0.804 805- 610 216 213 40 5.3 683.68 0.99 0.646 0.660 608- 472 209 202 40 5.0 488.55 0.75 0.742 0.916 468- 345 162 160 40 4.0 398.90 0.71 0.702 0.822 345- 146 156 155 40 3.9 234.12 0.48 0.781 1.086 145- -923 105 104 42 2.5 33.16 0.22 0.961 2.430 ------------------------------------------------------------------------------------------- 940403- -923 2301 2224 402 5.5 37416.86 4.29 0.166 0.159 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-1.26 475 460 40 11.5 83152.29 8.66 0.149 0.142 0.029 1.22-0.94 419 411 41 10.0 43217.58 4.77 0.199 0.198 0.056 0.94-0.81 329 312 42 7.4 24860.04 3.11 0.156 0.136 0.073 0.81-0.73 287 279 40 7.0 31492.74 3.65 0.192 0.196 0.081 0.73-0.68 235 228 41 5.6 16692.40 2.40 0.201 0.241 0.099 0.67-0.63 188 178 40 4.5 19720.97 2.58 0.143 0.129 0.105 0.63-0.59 146 139 40 3.5 10913.53 1.82 0.091 0.085 0.142 0.59-0.56 104 101 40 2.5 9616.63 1.68 0.108 0.109 0.138 0.56-0.53 72 70 41 1.7 8463.06 1.69 0.127 0.121 0.149 0.52-0.46 46 46 37 1.2 5715.88 1.49 0.594 0.665 0.148 ------------------------------------------------------------------------------------------------------ inf-0.46 2301 2224 402 5.5 37416.86 4.29 0.166 0.159 0.055 inf-0.65 1842 1783 224 8.0 43520.32 4.86 0.168 0.163 0.050 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-1.26 460 40 40 100.0 11.5 83152.29 25.29 0.149 0.011 1.22-0.94 411 41 41 100.0 10.0 43217.58 12.75 0.199 0.024 0.94-0.81 312 42 42 100.0 7.4 24860.04 8.03 0.156 0.034 0.81-0.73 279 40 40 100.0 7.0 31492.74 8.99 0.192 0.034 0.73-0.68 228 41 41 100.0 5.6 16692.40 5.68 0.201 0.050 0.67-0.63 178 44 40 90.9 4.5 19720.97 5.24 0.143 0.059 0.63-0.59 139 44 40 90.9 3.5 10913.53 3.18 0.091 0.081 0.59-0.56 101 54 40 74.1 2.5 9616.63 2.59 0.108 0.079 0.56-0.53 70 65 41 63.1 1.7 8463.06 2.06 0.127 0.128 0.52-0.46 46 200 37 18.5 1.2 5715.88 1.49 0.594 1.110 -------------------------------------------------------------------------------------------- inf-0.46 2224 613 402 65.6 5.5 37416.86 11.25 0.166 0.029 inf-0.65 1783 227 224 98.7 8.0 43520.32 13.20 0.168 0.023 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 -1.0 -2.0 1.0 -1.0 0.0 -1.0 -1.0 0.0 RRPPROF to HKL transformation matrix: -1.0 -1.0 -2.0 1.0 -1.0 0.0 -1.0 -1.0 0.0 No constraint UB - matrix: -0.008670 0.066461 -0.012666 ( 0.000016 0.000013 0.000018 ) -0.013357 -0.014280 -0.065093 ( 0.000016 0.000014 0.000019 ) -0.066270 -0.005982 0.014656 ( 0.000022 0.000018 0.000025 ) M - matrix: 0.004645 0.000011 0.000008 ( 0.000003 0.000002 0.000002 ) 0.000011 0.004657 0.000000 ( 0.000002 0.000002 0.000002 ) 0.000008 0.000000 0.004612 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.008670 0.066461 -0.012666 ( 0.000016 0.000013 0.000018 ) -0.013357 -0.014280 -0.065093 ( 0.000016 0.000014 0.000019 ) -0.066270 -0.005982 0.014656 ( 0.000022 0.000018 0.000025 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) unit cell: 10.407(3) 10.394(2) 10.444(3) 90.00(2) 90.10(2) 90.14(2) V = 1129.8(5) unit cell: 10.4150(7) 10.4150(7) 10.4150(7) 90.0 90.0 90.0 V = 1129.75(13) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.105) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - -23.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.056) PROFFIT INFO: signal sum: min=-580.0000 max=7903371.0000 PROFFIT INFO: signal sum lp corr: min=-607.3175 max=1115342.2273 PROFFIT INFO: background sum: min=116.0000 max=7453.0000 PROFFIT INFO: background sum sig2: min=348.0000 max=4924.0000 PROFFIT INFO: num of signal pixels: min=29 max=490 PROFFIT INFO: Inet: min=-971.7080 max=1784547.6250 PROFFIT INFO: sig(Inet): min=64.2045 max=24341.2070 PROFFIT INFO: Inet/sig(Inet): min=-1.66 max=199.93 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 424 1604 2398 2880 3098 3582 3878 4066 4360 4554 4602 Percent 9.2 34.9 52.1 62.6 67.3 77.8 84.3 88.4 94.7 99.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2301 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 2301 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1784548- 127694 230 397759.14 75.88 100.00 127308- 4034 230 28660.15 19.80 100.00 3996- 2051 230 2862.69 7.16 97.83 2050- 1232 230 1588.56 3.86 52.17 1231- 812 230 1001.92 2.13 9.57 811- 541 230 665.98 1.64 6.52 540- 322 230 430.91 1.30 7.39 321- 146 230 228.00 0.66 0.87 146- 8 230 72.38 0.26 0.00 8- -972 231 -141.66 -0.27 0.00 ------------------------------------------------------------------------------------ 1784548- -972 2301 43293.92 11.24 37.42 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 230 106413.43 15.00 70.43 1.64- 1.26 230 79380.56 20.61 56.09 1.26- 1.06 230 67812.22 20.70 68.70 1.06- 0.97 230 41877.33 11.82 28.70 0.97- 0.88 230 24702.36 8.99 45.65 0.88- 0.80 230 43651.04 12.42 34.78 0.80- 0.75 230 19466.34 6.09 21.30 0.75- 0.71 230 22489.13 7.23 16.96 0.71- 0.67 230 23341.89 7.63 25.65 0.67- 0.63 231 3975.87 1.93 6.06 ------------------------------------------------------------------------------------ 6.00- 0.63 2301 43293.92 11.24 37.42 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 12:57:21 2019 Sorting 2301 observations 42 unique observations with > 7.00 F2/sig(F2) 2301 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 24 230 Total number of frames 230 Maximum number of 42 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 2301 observations in 3 runs Run # start # end # total # 1 0 17 18 2 0 17 36 3 0 4 41 Total number of frames 41 555 observations > 7.00 F2/sig(F2) 555 observations in 3 runs Run # start # end # total # 1 0 17 18 2 0 16 35 3 0 3 39 Total number of frames 39 Removing 'redundancy=1' reflections Average redundancy: 11.4 (Out of 555 removed 6 = 549, unique = 48) 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 549 observations in 3 runs Run # start # end # total # 1 0 17 18 2 0 16 35 3 0 3 39 Total number of frames 39 48 unique data precomputed (should be 48) 48 unique data with 549 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 11.4 (Out of 549 removed 0 = 549, unique = 48) 48 unique data precomputed (should be 48) 48 unique data with 549 observations RMS deviation of equivalent data = 0.23876 Rint = 0.19574 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19296, wR= 0.25465 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08573, wR= 0.14546, Acormin=0.599, Acormax=1.312, Acor_av=1.029 F test: Probability=1.000, F= 5.016 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08991, wR= 0.14252, Acormin=0.505, Acormax=1.390, Acor_av=0.972 F test: Probability=0.000, F= 0.904 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08265, wR= 0.13808, Acormin=0.524, Acormax=1.349, Acor_av=0.954 F test: Probability=0.727, F= 1.056 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08317, wR= 0.13264, Acormin=0.439, Acormax=1.425, Acor_av=0.922 F test: Probability=0.655, F= 1.037 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08614, wR= 0.13070, Acormin=0.438, Acormax=1.332, Acor_av=0.889 F test: Probability=0.000, F= 0.952 Final absorption model (ne=2, no=0): Rint= 0.08573, Acormin=0.599, Acormax=1.312, Acor_av=1.029 Combined refinement in use Rint: 0.19786 There are 39 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 43 pars with 946 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.23876 Using Levenberg-Marquardt: 0.00010 New wR= 0.12404 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19574 with corrections 0.08261 Rint for all data: 0.19786 with corrections 0.08572 2 observations identified as outliers and rejected Cycle 2 wR= 0.10581 Using Levenberg-Marquardt: 0.00001 New wR= 0.09873 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.19333 with corrections 0.07148 Rint for all data: 0.19786 with corrections 0.07789 2 observations identified as outliers and rejected Cycle 3 wR= 0.08322 Using Levenberg-Marquardt: 0.00000 New wR= 0.07715 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18968 with corrections 0.06148 Rint for all data: 0.19786 with corrections 0.07206 0 observations identified as outliers and rejected Cycle 4 wR= 0.07715 Using Levenberg-Marquardt: 0.00000 New wR= 0.07710 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18968 with corrections 0.06179 Rint for all data: 0.19786 with corrections 0.07246 Final wR= 0.07710 Final frame scales: Min= 0.7231 Max= 1.2408 Final absorption correction factors: Amin= 0.7299 Amax= 1.3626 PROFFIT INFO: Inet (after scale3 abspack): min=-1066.7039 max=1225253.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=59.9770 max=23356.5176 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/103 2301 reflections read from tmp file 122 reflections are rejected (120 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 10 9 6 5 5 7 7 9 102 Initial Chi^2= 0.59583 Cycle 1, Chi^2= 1.02633 Current error model SIG(F2)^2 = 87.34*I_RAW + 5.32*I_BACK+(0.03975*)^2 Cycle 2, Chi^2= 1.02580 Current error model SIG(F2)^2 = 108.63*I_RAW + 2.61*I_BACK+(0.02503*)^2 Cycle 3, Chi^2= 1.00670 Current error model SIG(F2)^2 = 114.83*I_RAW + 2.16*I_BACK+(0.02342*)^2 Cycle 4, Chi^2= 0.99928 Current error model SIG(F2)^2 = 115.36*I_RAW + 2.23*I_BACK+(0.02356*)^2 Cycle 5, Chi^2= 1.00004 Current error model SIG(F2)^2 = 115.28*I_RAW + 2.22*I_BACK+(0.02356*)^2 Final Chi^2= 1.00004 Final error model SIG(F2)^2 = 115.28*I_RAW + 2.22*I_BACK+(0.02356*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1225253- 124677 230 379469.43 31.33 100.00 124092- 3771 230 29053.45 11.88 100.00 3756- 1997 230 2772.55 5.37 96.09 1985- 1181 230 1521.75 3.39 47.83 1180- 790 230 971.82 2.43 13.48 785- 530 230 659.21 2.05 7.39 529- 321 230 418.90 1.85 9.57 320- 141 230 227.74 1.31 0.87 141- 8 230 71.82 0.69 0.00 7- -1067 231 -145.49 -0.58 0.00 ------------------------------------------------------------------------------------ 1225253- -1067 2301 41484.02 5.97 37.51 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 230 100917.30 9.92 71.74 1.64- 1.26 230 76319.03 8.91 56.09 1.26- 1.06 230 66944.97 8.85 70.00 1.06- 0.97 230 38837.48 5.46 28.70 0.97- 0.88 230 23629.47 5.26 45.22 0.88- 0.80 230 42044.54 6.50 33.48 0.80- 0.75 230 19183.91 3.79 20.00 0.75- 0.71 230 20945.25 4.62 16.96 0.71- 0.67 230 22276.23 4.76 26.96 0.67- 0.63 231 3905.37 1.64 6.06 ------------------------------------------------------------------------------------ 6.00- 0.63 2301 41484.02 5.97 37.51 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 230 100917.30 9.92 71.74 6.00- 1.26 460 88618.17 9.42 63.91 6.00- 1.06 690 81393.77 9.23 65.94 6.00- 0.97 920 70754.69 8.28 56.63 6.00- 0.88 1150 61329.65 7.68 54.35 6.00- 0.80 1380 58115.46 7.48 50.87 6.00- 0.75 1610 52553.81 6.95 46.46 6.00- 0.71 1840 48602.74 6.66 42.77 6.00- 0.67 2070 45677.58 6.45 41.01 6.00- 0.63 2301 41484.02 5.97 37.51 ------------------------------------------------------------------------------------ 6.00- 0.63 2301 41484.02 5.97 37.51 Scale applied to data: s=0.816157 (maximum obs:1225253.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.072; Rsigma 0.038: data 2301 -> merged 162 With outlier rejection... Rint 0.061; Rsigma 0.038: data 2286 -> merged 162 Rejected total: 15, method kkm 12, method Blessing 3 Completeness direct cell (a, b, c) = (10.415, 10.415, 10.415), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626912, 6.013127 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.76 14 14 14.36 100.00 201 1.74 - 1.27 14 14 16.57 100.00 232 1.26 - 1.06 14 14 18.43 100.00 258 1.05 - 0.97 14 14 16.07 100.00 225 0.95 - 0.88 14 14 17.14 100.00 240 0.87 - 0.81 14 14 15.07 100.00 211 0.80 - 0.76 14 14 15.86 100.00 222 0.76 - 0.72 14 14 13.43 100.00 188 0.72 - 0.69 14 14 14.07 100.00 197 0.69 - 0.65 19 19 12.26 100.00 233 --------------------------------------------------------------- 7.37 - 0.65 145 145 15.22 100.00 2207 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 12:57:21 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.369438 7.367192 7.381632 120.2763 120.1020 89.6834 2224 Reflections read from file xs2212a.hkl 2145 Reflections used for space-group determination (up to diffraction limit of 0.65A); mean (I/sigma) = 4.41 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1084 1070 1078 1077 1616 1414 1419 2145 N (int>3sigma) = 0 110 109 153 101 186 299 305 455 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 24.7 27.7 25.9 Mean int/sigma = 0.0 1.3 1.3 1.8 1.3 1.5 4.2 4.7 4.4 Lattice type: P chosen Volume: 282.54 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 1.0000 Unitcell: 7.344 7.364 7.367 60.01 60.13 89.91 Niggli form: a.a = 53.929 b.b = 54.231 c.c = 54.271 b.c = 27.113 a.c = 26.945 a.b = 0.088 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.536 CUBIC F-lattice R(int) = 0.220 [ 1935] Vol = 1130.2 Cell: 10.408 10.392 10.449 90.02 90.11 90.16 Volume: 1130.16 Matrix:-1.0000 -1.0000 -2.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.526 TETRAGONAL I-lattice R(int) = 0.170 [ 1586] Vol = 565.1 Cell: 7.367 7.369 10.408 90.03 89.81 89.68 Volume: 565.08 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.349 TETRAGONAL I-lattice R(int) = 0.204 [ 1602] Vol = 565.1 Cell: 7.344 7.364 10.449 89.93 89.91 89.91 Volume: 565.08 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.330 ORTHORHOMBIC F-lattice R(int) = 0.170 [ 1577] Vol = 1130.2 Cell: 10.408 10.392 10.449 89.98 90.11 89.84 Volume: 1130.16 Matrix: 1.0000 1.0000 2.0000 1.0000 -1.0000 0.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.532 ORTHORHOMBIC I-lattice R(int) = 0.177 [ 1522] Vol = 565.1 Cell: 10.408 7.369 7.367 89.68 89.81 90.03 Volume: 565.08 Matrix: 1.0000 1.0000 2.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.090 ORTHORHOMBIC I-lattice R(int) = 0.203 [ 1548] Vol = 565.1 Cell: 7.344 7.364 10.449 90.07 90.09 89.91 Volume: 565.08 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.325 MONOCLINIC I-lattice R(int) = 0.102 [ 1164] Vol = 565.1 Cell: 7.367 10.392 7.382 90.10 90.22 90.13 Volume: 565.08 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.314 MONOCLINIC I-lattice R(int) = 0.167 [ 1155] Vol = 565.1 Cell: 7.369 10.408 7.367 90.19 90.32 90.03 Volume: 565.08 Matrix:-1.0000 0.0000 0.0000 1.0000 1.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.090 MONOCLINIC I-lattice R(int) = 0.160 [ 1097] Vol = 565.1 Cell: 7.364 7.344 10.449 89.91 90.07 90.09 Volume: 565.08 Matrix: 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.088 MONOCLINIC I-lattice R(int) = 0.201 [ 1182] Vol = 565.1 Cell: 7.344 7.364 10.449 89.93 90.09 90.09 Volume: 565.08 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.096 [ 495] Vol = 282.5 Cell: 7.344 7.364 7.367 60.01 60.13 89.91 Volume: 282.54 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 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 1078 0 1414 1416 2145 N (int>3sigma) = 0 0 0 0 153 0 299 316 455 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 24.7 26.8 25.9 Mean int/sigma = 0.0 0.0 0.0 0.0 1.8 0.0 4.2 4.4 4.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.125 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 11 11 157 403 N I>3s 0 0 0 88 0.1 0.1 0.0 1.6 0.6 0.6 0.2 2.4 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 0.220 1802 Fd-3m 1 1 227 C N N N N 37 2284 0.220 1859 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.408403 10.391541 10.449121 90.0175 90.1146 90.1602 ZERR 1.00 0.011870 0.006367 0.001112 0.0006 0.1236 0.0005 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1118791- 100220 277 268 27 9.9 332311.27 29.29 0.056 0.062 78370- 1695 439 436 27 16.1 5602.98 7.33 0.125 0.165 1628- 776 438 437 27 16.2 1160.76 2.69 0.245 0.297 762- 373 412 411 27 15.2 546.82 1.87 0.374 0.487 369- 60 392 391 27 14.5 229.23 1.15 0.558 0.897 56- -321 343 343 27 12.7 -2.29 0.15 0.959 3.273 ------------------------------------------------------------------------------------------- 1118791- -321 2301 2286 162 14.1 40386.33 5.90 0.061 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-1.27 437 431 27 16.0 88908.63 9.66 0.050 0.051 0.027 1.26-0.97 470 467 27 17.3 51084.94 6.96 0.047 0.054 0.034 0.97-0.81 431 429 27 15.9 35023.04 6.20 0.072 0.091 0.044 0.81-0.73 417 417 27 15.4 11563.60 2.86 0.093 0.105 0.067 0.73-0.67 336 334 27 12.4 28168.75 5.58 0.092 0.108 0.059 0.67-0.63 210 208 27 7.7 4286.55 1.73 0.216 0.158 0.132 ------------------------------------------------------------------------------------------------------ inf-0.63 2301 2286 162 14.1 40386.33 5.90 0.061 0.067 0.038 inf-0.65 2218 2205 144 15.3 41544.03 6.03 0.060 0.065 0.037 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-1.27 431 27 27 100.0 16.0 88908.63 37.11 0.050 0.011 1.26-0.97 467 27 27 100.0 17.3 51084.94 27.36 0.047 0.010 0.97-0.81 429 27 27 100.0 15.9 35023.04 24.83 0.072 0.013 0.81-0.73 417 27 27 100.0 15.4 11563.60 10.62 0.093 0.020 0.73-0.67 334 27 27 100.0 12.4 28168.75 20.46 0.092 0.018 0.67-0.63 208 27 27 100.0 7.7 4286.55 5.01 0.216 0.053 -------------------------------------------------------------------------------------------- inf-0.63 2286 162 162 100.0 14.1 40386.33 22.63 0.061 0.013 inf-0.65 2205 144 144 100.0 15.3 41544.03 23.28 0.060 0.012 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:04:01 2019) ID: 3668; threads 40; handles 811; mem 514796.00 (1204688.00)kB; time: 1w 4d 23h 14m 48s MEMORY INFO: Memory PF:282.0, Ph:666.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.7,peak PF: 700.2, WS: 470.7, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:284.0, Ph:667.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.5,peak PF: 700.2, WS: 472.5, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:04:01 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000101 0.000065 0.000100 ) 0.064809 0.092374 0.027273 ( 0.000113 0.000073 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000133 0.000085 0.000131 ) 7.38096 ( 0.00734 ) 7.36649 ( 0.00768 ) 7.42630 ( 0.00866 ) 120.52449 ( 0.11723 ) 120.40327 ( 0.11445 ) 89.27095 ( 0.08255 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:04:01 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000101 0.000065 0.000100 ) 0.064809 0.092374 0.027273 ( 0.000113 0.000073 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000133 0.000085 0.000131 ) M - matrix: 0.013828 0.004582 0.009194 ( 0.000026 0.000016 0.000022 ) 0.004582 0.013992 0.009354 ( 0.000016 0.000018 0.000018 ) 0.009194 0.009354 0.018489 ( 0.000022 0.000018 0.000035 ) unit cell: 7.381(7) 7.366(8) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | 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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb PROFFITPEAK info: 247 peaks in the peak location table UB fit with 38 obs out of 131 (total:131,skipped:0) (29.01%) UB - matrix: 0.086920 -0.045497 0.015286 ( 0.000208 0.000298 0.000586 ) 0.064723 0.092339 0.027914 ( 0.000160 0.000230 0.000452 ) 0.045474 0.057985 0.132131 ( 0.000191 0.000273 0.000537 ) M - matrix: 0.013812 0.004659 0.009144 ( 0.000045 0.000038 0.000069 ) 0.004659 0.013959 0.009544 ( 0.000038 0.000060 0.000069 ) 0.009144 0.009544 0.018471 ( 0.000069 0.000069 0.000145 ) unit cell: 7.36(2) 7.47(2) 7.46(3) 121.4(4) 119.5(4) 89.6(3) V = 287(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 38 obs out of 131 (total:131,skipped:0) (29.01%) UB - matrix: 0.086920 -0.045497 0.015286 ( 0.000208 0.000298 0.000586 ) 0.064723 0.092339 0.027914 ( 0.000160 0.000230 0.000452 ) 0.045474 0.057985 0.132131 ( 0.000191 0.000273 0.000537 ) M - matrix: 0.013812 0.004659 0.009144 ( 0.000045 0.000038 0.000069 ) 0.004659 0.013959 0.009544 ( 0.000038 0.000060 0.000069 ) 0.009144 0.009544 0.018471 ( 0.000069 0.000069 0.000145 ) unit cell: 7.36(2) 7.47(2) 7.46(3) 121.4(4) 119.5(4) 89.6(3) V = 287(2) OTKP changes: 30 1 1 1 OTKP changes: 30 1 1 1 OTKP changes: 30 1 1 1 UB - matrix: 0.087959 -0.044424 0.013200 ( 0.000071 0.000068 0.000111 ) 0.061734 0.094108 0.026039 ( 0.000064 0.000061 0.000100 ) 0.048603 0.056094 0.132830 ( 0.000082 0.000078 0.000128 ) M - matrix: 0.013910 0.004629 0.009225 ( 0.000017 0.000011 0.000017 ) 0.004629 0.013976 0.009315 ( 0.000011 0.000016 0.000017 ) 0.009225 0.009315 0.018496 ( 0.000017 0.000017 0.000034 ) UB fit with 124 obs out of 131 (total:131,skipped:0) (94.66%) unit cell: 7.351(6) 7.361(6) 7.378(8) 120.22(10) 119.86(9) 89.89(6) V = 282.2(4) UB fit with 124 obs out of 131 (total:131,skipped:0) (94.66%) UB - matrix: 0.087959 -0.044424 0.013200 ( 0.000071 0.000068 0.000111 ) 0.061734 0.094108 0.026039 ( 0.000064 0.000061 0.000100 ) 0.048603 0.056094 0.132830 ( 0.000082 0.000078 0.000128 ) M - matrix: 0.013910 0.004629 0.009225 ( 0.000017 0.000011 0.000017 ) 0.004629 0.013976 0.009315 ( 0.000011 0.000016 0.000017 ) 0.009225 0.009315 0.018496 ( 0.000017 0.000017 0.000034 ) unit cell: 7.351(6) 7.361(6) 7.378(8) 120.22(10) 119.86(9) 89.89(6) V = 282.2(4) OTKP changes: 46 1 1 1 OTKP changes: 46 1 1 1 UB - matrix: 0.087663 -0.044322 0.013251 ( 0.000069 0.000067 0.000109 ) 0.061710 0.093786 0.026118 ( 0.000062 0.000060 0.000098 ) 0.048294 0.055927 0.132325 ( 0.000081 0.000078 0.000126 ) M - matrix: 0.013825 0.004603 0.009164 ( 0.000016 0.000011 0.000017 ) 0.004603 0.013888 0.009263 ( 0.000011 0.000015 0.000016 ) 0.009164 0.009263 0.018368 ( 0.000017 0.000016 0.000034 ) UB fit with 124 obs out of 131 (total:131,skipped:0) (94.66%) unit cell: 7.374(6) 7.388(6) 7.407(8) 120.27(10) 119.85(9) 89.89(6) V = 285.1(4) 131 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Run 3 Omega scan: (-48.000 - 2.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.256) HKL list info: 727 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087663 -0.044322 0.013251 ( 0.000069 0.000067 0.000109 ) 0.061710 0.093786 0.026118 ( 0.000062 0.000060 0.000098 ) 0.048294 0.055927 0.132325 ( 0.000081 0.000078 0.000126 ) M - matrix: 0.013825 0.004603 0.009164 ( 0.000016 0.000011 0.000017 ) 0.004603 0.013888 0.009263 ( 0.000011 0.000015 0.000016 ) 0.009164 0.009263 0.018368 ( 0.000017 0.000016 0.000034 ) UB fit with 124 obs out of 131 (total:131,skipped:0) (94.66%) unit cell: 7.374(6) 7.388(6) 7.407(8) 120.27(10) 119.85(9) 89.89(6) V = 285.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 124 obs out of 131 (total:131,skipped:0) (94.66%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb 0 of 112 peaks identified as outliers and rejected 112 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 112 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 112 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.17- 2.39 | 11 | 0.847 ( 0.099) | 0.857 ( 0.143) | 1.136 ( 0.430) | 2.38- 1.83 | 11 | 0.890 ( 0.105) | 0.893 ( 0.141) | 1.030 ( 0.525) | 1.77- 1.65 | 11 | 0.900 ( 0.089) | 0.934 ( 0.121) | 0.785 ( 0.203) | 1.58- 1.36 | 11 | 0.945 ( 0.077) | 0.962 ( 0.120) | 0.797 ( 0.273) | 1.36- 1.20 | 11 | 0.947 ( 0.083) | 0.965 ( 0.132) | 0.990 ( 0.542) | 1.19- 1.09 | 11 | 0.970 ( 0.053) | 0.986 ( 0.128) | 0.824 ( 0.333) | 1.06- 0.92 | 11 | 0.997 ( 0.059) | 1.031 ( 0.096) | 0.949 ( 0.316) | 0.89- 0.79 | 11 | 0.990 ( 0.048) | 0.944 ( 0.103) | 1.058 ( 0.498) | 0.79- 0.70 | 11 | 0.982 ( 0.044) | 0.924 ( 0.062) | 1.301 ( 0.529) | 0.70- 0.63 | 13 | 0.963 ( 0.055) | 0.851 ( 0.078) | 1.251 ( 0.492) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.17- 0.63 | 112 | 0.943 ( 0.087) | 0.933 ( 0.127) | 1.016 ( 0.465) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 112 obs out of 112 (total:112,skipped:0) (100.00%) UB - matrix: 0.087839 -0.044284 0.013350 ( 0.000046 0.000046 0.000072 ) 0.061769 0.093770 0.026167 ( 0.000033 0.000033 0.000052 ) 0.048324 0.055610 0.132504 ( 0.000054 0.000054 0.000086 ) M - matrix: 0.013866 0.004590 0.009192 ( 0.000010 0.000007 0.000011 ) 0.004590 0.013846 0.009231 ( 0.000007 0.000009 0.000010 ) 0.009192 0.009231 0.018420 ( 0.000011 0.000010 0.000023 ) unit cell: 7.363(4) 7.387(3) 7.387(5) 120.13(6) 119.89(6) 89.90(4) V = 284.3(3) OTKP changes: 112 1 1 1 OTKP changes: 112 1 1 1 UB - matrix: 0.087890 -0.044338 0.013408 ( 0.000037 0.000037 0.000058 ) 0.061859 0.093929 0.026131 ( 0.000032 0.000032 0.000051 ) 0.048647 0.055909 0.132849 ( 0.000040 0.000040 0.000063 ) M - matrix: 0.013918 0.004633 0.009258 ( 0.000008 0.000006 0.000009 ) 0.004633 0.013914 0.009287 ( 0.000006 0.000008 0.000008 ) 0.009258 0.009287 0.018511 ( 0.000009 0.000008 0.000017 ) UB fit with 112 obs out of 112 (total:112,skipped:0) (100.00%) unit cell: 7.360(3) 7.373(3) 7.379(4) 120.13(5) 119.96(5) 89.93(3) V = 282.9(2) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 2.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.081) HKL list info: 727 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087890 -0.044338 0.013408 ( 0.000037 0.000037 0.000058 ) 0.061859 0.093929 0.026131 ( 0.000032 0.000032 0.000051 ) 0.048647 0.055909 0.132849 ( 0.000040 0.000040 0.000063 ) M - matrix: 0.013918 0.004633 0.009258 ( 0.000008 0.000006 0.000009 ) 0.004633 0.013914 0.009287 ( 0.000006 0.000008 0.000008 ) 0.009258 0.009287 0.018511 ( 0.000009 0.000008 0.000017 ) UB fit with 112 obs out of 112 (total:112,skipped:0) (100.00%) unit cell: 7.360(3) 7.373(3) 7.379(4) 120.13(5) 119.96(5) 89.93(3) V = 282.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 112 obs out of 112 (total:112,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb 0 of 115 peaks identified as outliers and rejected 115 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 115 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 115 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 12 | 0.865 ( 0.087) | 0.880 ( 0.117) | 1.048 ( 0.462) | 2.38- 1.76 | 12 | 0.866 ( 0.118) | 0.854 ( 0.168) | 0.967 ( 0.413) | 1.76- 1.58 | 12 | 0.919 ( 0.086) | 0.968 ( 0.107) | 0.772 ( 0.196) | 1.58- 1.35 | 12 | 0.959 ( 0.080) | 0.981 ( 0.126) | 0.827 ( 0.248) | 1.35- 1.16 | 12 | 0.921 ( 0.078) | 0.889 ( 0.153) | 0.890 ( 0.536) | 1.16- 1.01 | 12 | 0.986 ( 0.051) | 1.011 ( 0.094) | 0.984 ( 0.298) | 1.00- 0.88 | 12 | 0.961 ( 0.107) | 0.989 ( 0.090) | 0.922 ( 0.360) | 0.88- 0.73 | 12 | 1.007 ( 0.046) | 0.952 ( 0.103) | 1.222 ( 0.516) | 0.73- 0.68 | 12 | 0.966 ( 0.035) | 0.892 ( 0.073) | 1.254 ( 0.517) | 0.68- 0.63 | 7 | 0.960 ( 0.064) | 0.845 ( 0.074) | 1.151 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 115 | 0.940 ( 0.092) | 0.930 ( 0.129) | 0.997 ( 0.445) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.7 | 58 | 0.974 ( 0.040) | 1.011 ( 0.084) | 1.132 ( 0.439) | 10.7-15.0 | 58 | 0.984 ( 0.044) | 1.043 ( 0.067) | 1.167 ( 0.520) | 15.1-19.2 | 58 | 0.995 ( 0.273) | 1.019 ( 0.110) | 1.259 ( 1.380) | 19.3-23.6 | 58 | 0.949 ( 0.053) | 0.989 ( 0.079) | 0.941 ( 0.419) | 23.7-27.2 | 58 | 0.956 ( 0.066) | 0.992 ( 0.096) | 0.958 ( 0.440) | 27.3-32.9 | 58 | 0.936 ( 0.094) | 0.941 ( 0.120) | 0.943 ( 0.476) | 33.1-36.4 | 58 | 0.921 ( 0.192) | 0.896 ( 0.121) | 1.110 ( 0.733) | 36.5-38.9 | 58 | 0.865 ( 0.093) | 0.825 ( 0.103) | 1.000 ( 0.513) | 39.0-41.8 | 58 | 0.888 ( 0.095) | 0.830 ( 0.128) | 1.091 ( 0.470) | 41.9-50.1 | 59 | 0.868 ( 0.107) | 0.786 ( 0.119) | 1.000 ( 0.509) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 581 | 0.934 ( 0.134) | 0.933 ( 0.137) | 1.060 ( 0.659) | Fitted profile normalization line parameters e1 dimension: a=-0.0035 b=1.14 e2 dimension: a=-0.0077 b=1.27 e3 dimension: a=0.0039 b=0.97 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:04:10 2019 PROFFITMAIN - Started at Wed Aug 21 13:04:10 2019 OTKP changes: 288 2 2 3 OTKP changes: 288 2 2 3 OTKP changes: 288 2 2 3 UB - matrix: 0.087642 -0.046072 0.016922 ( 0.000092 0.000062 0.000091 ) 0.063803 0.092472 0.027028 ( 0.000103 0.000070 0.000102 ) 0.045547 0.057732 0.132205 ( 0.000109 0.000074 0.000108 ) M - matrix: 0.013826 0.004492 0.009229 ( 0.000023 0.000014 0.000019 ) 0.004492 0.014007 0.009352 ( 0.000014 0.000016 0.000016 ) 0.009229 0.009352 0.018495 ( 0.000019 0.000016 0.000029 ) UB fit with 327 obs out of 581 (total:581,skipped:0) (56.28%) unit cell: 7.388(7) 7.365(7) 7.429(7) 120.71(10) 120.38(10) 88.92(8) V = 283.7(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 202 obs out of 212 (total:212,skipped:0) (95.28%) UB - matrix: 0.087530 -0.046199 0.017267 ( 0.000105 0.000065 0.000097 ) 0.064763 0.092391 0.027185 ( 0.000089 0.000055 0.000082 ) 0.045934 0.057793 0.132186 ( 0.000107 0.000066 0.000099 ) M - matrix: 0.013966 0.004594 0.009344 ( 0.000024 0.000014 0.000018 ) 0.004594 0.014011 0.009353 ( 0.000014 0.000014 0.000014 ) 0.009344 0.009353 0.018510 ( 0.000018 0.000014 0.000027 ) unit cell: 7.376(7) 7.362(6) 7.434(7) 120.48(9) 120.51(10) 89.21(7) V = 283.1(4) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.088) HKL list info: 1290 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087479 -0.046164 0.017368 ( 0.000099 0.000062 0.000092 ) 0.064783 0.092381 0.027261 ( 0.000087 0.000054 0.000080 ) 0.045703 0.057853 0.132165 ( 0.000104 0.000065 0.000097 ) M - matrix: 0.013938 0.004590 0.009326 ( 0.000023 0.000013 0.000018 ) 0.004590 0.014012 0.009363 ( 0.000013 0.000014 0.000013 ) 0.009326 0.009363 0.018513 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.380(6) 7.365(6) 7.433(6) 120.53(9) 120.46(9) 89.22(7) V = 283.3(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118089 0.039060 0.078758 ( 0.000074 0.000046 0.000068 ) 0.000079 0.111623 0.056290 ( 0.000078 0.000049 0.000072 ) -0.000053 -0.000056 0.095478 ( 0.000089 0.000056 0.000083 ) M - matrix: 0.013945 0.004621 0.009300 ( 0.000017 0.000011 0.000014 ) 0.004621 0.013985 0.009354 ( 0.000011 0.000011 0.000011 ) 0.009300 0.009354 0.018487 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.369(5) 7.374(5) 7.425(8) 120.47(9) 120.25(9) 89.48(6) V = 283.5(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) UB - matrix: 0.087890 -0.044337 0.013396 ( 0.000035 0.000034 0.000055 ) 0.061861 0.093939 0.026136 ( 0.000032 0.000031 0.000050 ) 0.048655 0.055902 0.132879 ( 0.000039 0.000038 0.000061 ) M - matrix: 0.013919 0.004634 0.009259 ( 0.000008 0.000006 0.000008 ) 0.004634 0.013915 0.009289 ( 0.000006 0.000008 0.000008 ) 0.009259 0.009289 0.018519 ( 0.000008 0.000008 0.000016 ) unit cell: 7.359(3) 7.373(3) 7.376(4) 120.13(5) 119.96(5) 89.94(3) V = 282.8(2) OTKP changes: 115 1 1 1 OTKP changes: 115 1 1 1 OTKP changes: 115 1 1 1 OTKP changes: 115 1 1 1 OTKP changes: 115 1 1 1 OTKP changes: 115 1 1 1 Run 3 Omega scan: (-48.000 - 2.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.081) HKL list info: 708 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087890 -0.044337 0.013396 ( 0.000035 0.000034 0.000055 ) 0.061861 0.093939 0.026136 ( 0.000032 0.000031 0.000050 ) 0.048655 0.055902 0.132879 ( 0.000039 0.000038 0.000061 ) M - matrix: 0.013919 0.004634 0.009259 ( 0.000008 0.000006 0.000008 ) 0.004634 0.013915 0.009289 ( 0.000006 0.000008 0.000008 ) 0.009259 0.009289 0.018519 ( 0.000008 0.000008 0.000016 ) UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) unit cell: 7.359(3) 7.373(3) 7.376(4) 120.13(5) 119.96(5) 89.94(3) V = 282.8(2) 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! *** Best per run unit cell (run 3) ******* UB - matrix: 0.087890 -0.044337 0.013396 ( 0.000035 0.000034 0.000055 ) 0.061861 0.093939 0.026136 ( 0.000032 0.000031 0.000050 ) 0.048655 0.055902 0.132879 ( 0.000039 0.000038 0.000061 ) M - matrix: 0.013919 0.004634 0.009259 ( 0.000008 0.000006 0.000008 ) 0.004634 0.013915 0.009289 ( 0.000006 0.000008 0.000008 ) 0.009259 0.009289 0.018519 ( 0.000008 0.000008 0.000016 ) UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) unit cell: 7.359(3) 7.373(3) 7.376(4) 120.13(5) 119.96(5) 89.94(3) V = 282.8(2) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117969 0.039086 0.078682 ( 0.000029 0.000029 0.000035 ) 0.000080 0.111541 0.056252 ( 0.000030 0.000029 0.000036 ) -0.000023 -0.000132 0.096043 ( 0.000034 0.000034 0.000041 ) M - matrix: 0.013917 0.004620 0.009284 ( 0.000007 0.000005 0.000006 ) 0.004620 0.013969 0.009337 ( 0.000005 0.000007 0.000006 ) 0.009284 0.009337 0.018580 ( 0.000006 0.000006 0.000011 ) UB fit with 576 obs out of 581 (total:581,skipped:0) (99.14%) unit cell: 7.364(2) 7.364(2) 7.379(4) 120.27(4) 120.08(4) 89.72(3) V = 282.21(18) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 67 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof 2560 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:04:14 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.088) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 2.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.081) PROFFIT INFO: signal sum: min=-557.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-617.4496 max=1123819.5642 PROFFIT INFO: background sum: min=163.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=405.0000 max=5234.0000 PROFFIT INFO: num of signal pixels: min=37 max=523 PROFFIT INFO: Inet: min=-987.9194 max=1798111.3750 PROFFIT INFO: sig(Inet): min=63.3237 max=24261.9844 PROFFIT INFO: Inet/sig(Inet): min=-1.64 max=202.94 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 224 902 1337 1599 1714 1990 2158 2262 2427 2532 2560 Percent 8.8 35.2 52.2 62.5 67.0 77.7 84.3 88.4 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2560 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 2560 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1798111- 126913 256 403086.19 76.51 100.00 126173- 4053 256 28518.72 19.75 100.00 4031- 2123 256 2921.25 7.30 98.44 2116- 1227 256 1606.77 3.91 52.34 1225- 816 256 1000.84 2.16 10.94 815- 536 256 669.51 1.65 6.25 535- 317 256 424.55 1.27 6.25 317- 149 256 227.10 0.66 1.17 147- 17 256 76.75 0.27 0.00 17- -988 256 -145.63 -0.28 0.00 ------------------------------------------------------------------------------------ 1798111- -988 2560 43838.60 11.32 37.54 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 256 109515.46 18.15 69.92 1.59- 1.26 256 77418.46 18.62 56.25 1.26- 1.04 256 59121.45 16.41 52.34 1.04- 0.92 256 26661.30 8.86 37.50 0.92- 0.83 256 40894.78 11.95 33.98 0.83- 0.75 256 33508.77 10.42 35.16 0.75- 0.69 256 37294.47 11.04 31.64 0.69- 0.64 256 22701.35 7.13 21.88 0.64- 0.58 256 13674.15 4.92 18.75 0.58- 0.46 256 17595.83 5.72 17.97 ------------------------------------------------------------------------------------ 6.55- 0.46 2560 43838.60 11.32 37.54 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:04:14 2019 Sorting 2560 observations 76 unique observations with > 7.00 F2/sig(F2) 2560 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 49 255 Total number of frames 255 Maximum number of 76 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 2560 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 12 65 Total number of frames 65 618 observations > 7.00 F2/sig(F2) 618 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 12 65 Total number of frames 65 Removing 'redundancy=1' reflections Average redundancy: 5.4 (Out of 618 removed 39 = 579, unique = 108) 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 579 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 12 65 Total number of frames 65 108 unique data precomputed (should be 108) 108 unique data with 579 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.4 (Out of 579 removed 0 = 579, unique = 108) 108 unique data precomputed (should be 108) 108 unique data with 579 observations RMS deviation of equivalent data = 0.38305 Rint = 0.34544 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.34544, wR= 0.46832 Trying model 1 (ne=2, no=0)... Results: Rint= 0.23796, wR= 0.33545, Acormin=0.491, Acormax=1.568, Acor_av=0.973 F test: Probability=1.000, F= 2.085 Trying model 2 (ne=2, no=1)... Results: Rint= 0.24620, wR= 0.34238, Acormin=0.239, Acormax=1.684, Acor_av=0.870 F test: Probability=0.000, F= 0.928 Trying model 3 (ne=4, no=0)... Results: Rint= 0.23713, wR= 0.31987, Acormin=0.435, Acormax=1.888, Acor_av=0.903 F test: Probability=0.000, F= 0.988 Trying model 4 (ne=4, no=1)... Results: Rint= 0.24707, wR= 0.32665, Acormin=0.201, Acormax=1.846, Acor_av=0.839 F test: Probability=0.000, F= 0.904 Trying model 5 (ne=4, no=3)... Results: Rint= 0.26542, wR= 0.30961, Acormin=0.148, Acormax=1.662, Acor_av=0.697 F test: Probability=0.000, F= 0.771 Trying model 6 (ne=6, no=0)... Results: Rint= 0.24369, wR= 0.29626, Acormin=0.209, Acormax=2.177, Acor_av=0.824 F test: Probability=0.000, F= 0.909 Trying model 7 (ne=6, no=1)... Results: Rint= 0.24289, wR= 0.29752, Acormin=0.051, Acormax=2.187, Acor_av=0.799 F test: Probability=0.000, F= 0.908 Trying model 8 (ne=6, no=3)... Results: Rint= 0.24871, wR= 0.27684, Acormin=0.040, Acormax=1.849, Acor_av=0.680 F test: Probability=0.000, F= 0.853 Trying model 9 (ne=6, no=5)... Results: Rint= 0.25527, wR= 0.28844, Acormin=-0.166, Acormax=2.166, Acor_av=0.375 F test: Probability=0.000, F= 0.789 Trying model 10 (ne=8, no=0)... Results: Rint= 0.24884, wR= 0.30391, Acormin=0.059, Acormax=2.553, Acor_av=0.690 F test: Probability=0.000, F= 0.838 Trying model 11 (ne=8, no=1)... Results: Rint= 0.34193, wR= 0.39785, Acormin=-0.175, Acormax=1.793, Acor_av=0.420 F test: Probability=0.000, F= 0.441 Trying model 12 (ne=8, no=3)... Results: Rint= 0.28438, wR= 0.30324, Acormin=-0.010, Acormax=0.125, Acor_av=0.046 F test: Probability=0.000, F= 0.627 Trying model 13 (ne=8, no=5)... Results: Rint= 0.21521, wR= 0.23374, Acormin=-0.004, Acormax=0.234, Acor_av=0.059 F test: Probability=0.744, F= 1.065 Trying model 14 (ne=8, no=7)... Results: Rint= 0.15202, wR= 0.18907, Acormin=0.006, Acormax=0.190, Acor_av=0.063 F test: Probability=1.000, F= 2.056 Final absorption model (ne=2, no=0): Rint= 0.23796, Acormin=0.491, Acormax=1.568, Acor_av=0.973 Combined refinement in use Rint: 0.36028 There are 65 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 69 pars with 2415 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.38305 Using Levenberg-Marquardt: 0.00010 New wR= 0.21500 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34544 with corrections 0.18164 Rint for all data: 0.36028 with corrections 0.19831 0 observations identified as outliers and rejected Cycle 2 wR= 0.21500 Using Levenberg-Marquardt: 0.00001 New wR= 0.21002 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34544 with corrections 0.17837 Rint for all data: 0.36028 with corrections 0.19512 0 observations identified as outliers and rejected Cycle 3 wR= 0.21002 Using Levenberg-Marquardt: 0.00000 New wR= 0.20628 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34544 with corrections 0.17735 Rint for all data: 0.36028 with corrections 0.19410 0 observations identified as outliers and rejected Cycle 4 wR= 0.20628 Using Levenberg-Marquardt: 0.00000 New wR= 0.20705 Using Levenberg-Marquardt: 0.00000 New wR= 0.20705 Using Levenberg-Marquardt: 0.00001 New wR= 0.20704 Using Levenberg-Marquardt: 0.00010 New wR= 0.20704 Using Levenberg-Marquardt: 0.00100 New wR= 0.20695 Using Levenberg-Marquardt: 0.01000 New wR= 0.20643 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34544 with corrections 0.17801 Rint for all data: 0.36028 with corrections 0.19473 Final wR= 0.20643 Final frame scales: Min= 0.5691 Max= 1.8181 Final absorption correction factors: Amin= 0.4941 Amax= 1.5726 PROFFIT INFO: Inet (after scale3 abspack): min=-1621.1465 max=1457633.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=43.4492 max=25379.4512 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/103 2560 reflections read from tmp file 711 reflections are rejected (619 as outliers, 92 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 51 60 45 39 30 26 25 16 43 Initial Chi^2= 2.47916 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.78615 Current error model SIG(F2)^2 = 530.71*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 417.22*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 417.22*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1457634- 115284 256 365990.19 32.02 100.00 113120- 4052 256 25554.88 6.80 82.42 4048- 1996 256 2688.86 2.72 30.08 1994- 1161 256 1534.55 1.97 16.41 1158- 732 256 924.65 1.38 2.73 731- 487 256 606.57 1.14 0.39 486- 293 256 381.68 1.01 0.39 292- 137 256 211.51 0.82 0.39 136- 15 256 69.72 0.47 0.00 15- -1621 256 -172.49 -0.34 0.00 ------------------------------------------------------------------------------------ 1457634- -1621 2560 39779.01 4.80 23.28 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 256 105577.05 11.51 54.30 1.59- 1.26 256 74182.70 8.00 37.50 1.26- 1.04 256 52077.96 6.54 33.20 1.04- 0.92 256 30390.41 3.30 16.02 0.92- 0.83 256 34000.18 4.24 18.75 0.83- 0.75 256 31134.28 3.72 17.58 0.75- 0.69 256 29579.62 3.93 17.97 0.69- 0.64 256 18012.81 2.64 12.89 0.64- 0.58 256 11027.87 1.97 11.33 0.58- 0.46 256 11807.24 2.15 13.28 ------------------------------------------------------------------------------------ 6.55- 0.46 2560 39779.01 4.80 23.28 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 256 105577.05 11.51 54.30 6.55- 1.26 512 89879.88 9.75 45.90 6.55- 1.04 768 77279.24 8.68 41.67 6.55- 0.92 1024 65557.03 7.34 35.25 6.55- 0.83 1280 59245.66 6.72 31.95 6.55- 0.75 1536 54560.43 6.22 29.56 6.55- 0.69 1792 50991.74 5.89 27.90 6.55- 0.64 2048 46869.38 5.48 26.03 6.55- 0.58 2304 42886.99 5.09 24.39 6.55- 0.46 2560 39779.01 4.80 23.28 ------------------------------------------------------------------------------------ 6.55- 0.46 2560 39779.01 4.80 23.28 Scale applied to data: s=0.686043 (maximum obs:1457633.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.195; Rsigma 0.050: data 2560 -> merged 434 With outlier rejection... Rint 0.174; Rsigma 0.050: data 2490 -> merged 434 Rejected total: 70, method kkm 62, method Blessing 8 Completeness direct cell (a, b, c) = (6.559, 6.559, 6.559), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.457008, 6.559296 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.38 - 1.59 22 22 12.82 100.00 282 1.55 - 1.22 22 22 12.14 100.00 267 1.20 - 1.02 22 22 10.82 100.00 238 1.02 - 0.92 22 22 9.41 100.00 207 0.92 - 0.84 22 22 8.91 100.00 196 0.84 - 0.79 22 22 7.41 100.00 163 0.79 - 0.75 22 22 7.55 100.00 166 0.75 - 0.71 22 22 6.18 100.00 136 0.71 - 0.69 22 22 6.09 100.00 134 0.68 - 0.65 26 29 5.65 89.66 147 --------------------------------------------------------------- 7.38 - 0.65 224 227 8.64 98.68 1936 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:04:15 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.364215 7.364421 7.379201 120.2659 120.0778 89.7162 2490 Reflections read from file xs2212a.hkl 2490 Reflections used for space-group determination (up to diffraction limit of 0.58A); mean (I/sigma) = 4.66 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1261 1248 1255 1243 1882 1652 1668 2490 N (int>3sigma) = 0 143 149 200 137 246 374 384 559 Mean intensity = 0.0 0.9 0.8 1.2 0.8 1.0 25.0 27.5 26.0 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.4 4.9 4.7 Lattice type: P chosen Volume: 282.21 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 Unitcell: 7.342 7.363 7.363 60.01 89.90 60.11 Niggli form: a.a = 53.908 b.b = 54.207 c.c = 54.214 b.c = 27.093 a.c = 0.096 a.b = 26.941 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.377 CUBIC F-lattice R(int) = 0.221 [ 2253] Vol = 1128.8 Cell: 10.407 10.440 10.389 90.00 89.84 89.87 Volume: 1128.84 Matrix: 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.194 RHOMBOHEDRAL R-lattice R(int) = 0.199 [ 1824] Vol = 846.6 Cell: 7.364 7.342 18.065 89.86 90.22 119.92 Volume: 846.63 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 -1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.194 RHOMBOHEDRAL R-lattice R(int) = 0.196 [ 573] Vol = 846.6 Trigonal Cell: 7.364 7.342 18.065 89.86 90.22 119.92 Volume: 846.63 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 -1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.499 ORTHORHOMBIC I-lattice R(int) = 0.171 [ 1811] Vol = 564.4 Cell: 7.364 10.407 7.364 89.79 89.72 90.02 Volume: 564.42 Matrix: 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.393 MONOCLINIC I-lattice R(int) = 0.127 [ 1296] Vol = 564.4 Cell: 10.407 7.364 7.364 90.28 90.21 90.02 Volume: 564.42 Matrix:-1.0000 -1.0000 -2.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.097 MONOCLINIC I-lattice R(int) = 0.164 [ 1319] Vol = 564.4 Cell: 7.363 7.342 10.440 89.91 90.09 90.10 Volume: 564.42 Matrix: 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.107 [ 588] Vol = 282.2 Cell: 7.342 7.363 7.363 60.01 89.90 60.11 Volume: 282.21 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 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 1255 0 1660 1654 2490 N (int>3sigma) = 0 0 0 0 200 0 387 387 559 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 26.2 27.0 26.0 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.8 4.7 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.781 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 182 475 N I>3s 0 0 0 116 0.1 0.1 -0.0 1.7 0.6 0.6 0.1 2.5 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 0.221 2099 Fd-3m 1 1 227 C N N N N 37 2284 0.221 2162 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.407446 10.440480 10.388893 89.9984 89.8373 89.8703 ZERR 1.00 0.010810 0.001012 0.005813 0.0011 0.0006 0.1113 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 959763- 103070 276 254 43 5.9 348436.37 31.07 0.156 0.155 97031- 2808 297 282 43 6.6 14224.56 4.70 0.321 0.197 2707- 1488 439 429 43 10.0 2025.11 2.14 0.825 0.945 1455- 1034 371 365 43 8.5 1175.13 1.47 0.764 0.841 1015- 784 272 268 43 6.2 838.89 1.17 0.684 0.726 775- 584 236 232 43 5.4 654.16 0.97 0.653 0.699 583- 448 231 223 43 5.2 469.83 0.80 0.721 0.840 447- 308 168 168 43 3.9 381.92 0.76 0.691 0.891 304- 137 150 150 43 3.5 220.42 0.49 0.860 1.231 137- -580 120 119 47 2.5 38.46 0.23 0.969 2.054 ------------------------------------------------------------------------------------------- 959763- -580 2560 2490 434 5.7 37909.65 4.66 0.174 0.170 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-1.22 565 549 44 12.5 79664.03 9.04 0.169 0.173 0.026 1.20-0.93 443 434 43 10.1 45696.87 5.23 0.194 0.185 0.049 0.92-0.80 376 362 44 8.2 32096.81 3.96 0.160 0.149 0.068 0.79-0.71 315 309 45 6.9 29579.72 3.73 0.195 0.197 0.075 0.71-0.65 269 258 44 5.9 10944.65 2.04 0.159 0.124 0.106 0.65-0.61 199 194 43 4.5 13450.83 2.23 0.172 0.194 0.112 0.61-0.57 163 158 43 3.7 12662.76 2.17 0.129 0.132 0.119 0.57-0.54 108 104 46 2.3 17855.71 2.99 0.166 0.151 0.104 0.54-0.51 78 78 43 1.8 6251.86 1.46 0.139 0.134 0.164 0.51-0.46 44 44 39 1.1 6575.24 1.62 0.790 0.907 0.128 ------------------------------------------------------------------------------------------------------ inf-0.46 2560 2490 434 5.7 37909.65 4.66 0.174 0.170 0.050 inf-0.65 1993 1936 224 8.6 45023.09 5.35 0.176 0.172 0.045 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-1.22 549 44 44 100.0 12.5 79664.03 27.52 0.169 0.009 1.20-0.93 434 43 43 100.0 10.1 45696.87 14.79 0.194 0.022 0.92-0.80 362 44 44 100.0 8.2 32096.81 10.37 0.160 0.031 0.79-0.71 309 45 45 100.0 6.9 29579.72 9.80 0.195 0.032 0.71-0.65 258 45 44 97.8 5.9 10944.65 4.51 0.159 0.051 0.65-0.61 194 46 43 93.5 4.5 13450.83 5.17 0.172 0.070 0.61-0.57 158 54 43 79.6 3.7 12662.76 3.96 0.129 0.064 0.57-0.54 104 52 46 88.5 2.3 17855.71 4.76 0.166 0.064 0.54-0.51 78 71 43 60.6 1.8 6251.86 1.93 0.139 0.107 0.51-0.46 44 169 39 23.1 1.1 6575.24 1.62 0.790 1.656 -------------------------------------------------------------------------------------------- inf-0.46 2490 613 434 70.8 5.7 37909.65 12.78 0.174 0.028 inf-0.65 1936 227 224 98.7 8.6 45023.09 15.25 0.176 0.021 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 2.0 -1.0 -1.0 0.0 1.0 -1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 2.0 -1.0 -1.0 0.0 1.0 -1.0 0.0 No constraint UB - matrix: 0.008649 -0.012719 0.066477 ( 0.000015 0.000016 0.000013 ) 0.013317 -0.065140 -0.014298 ( 0.000016 0.000016 0.000013 ) 0.066279 0.014596 -0.005963 ( 0.000020 0.000021 0.000017 ) M - matrix: 0.004645 -0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) -0.000010 0.004618 -0.000001 ( 0.000002 0.000003 0.000002 ) -0.000011 -0.000001 0.004659 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: 0.008649 -0.012719 0.066477 ( 0.000015 0.000016 0.000013 ) 0.013317 -0.065140 -0.014298 ( 0.000016 0.000016 0.000013 ) 0.066279 0.014596 -0.005963 ( 0.000020 0.000021 0.000017 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) unit cell: 10.407(3) 10.438(3) 10.391(2) 89.985(19) 89.869(19) 89.88(2) V = 1128.8(5) unit cell: 10.4121(6) 10.4121(6) 10.4121(6) 90.0 90.0 90.0 V = 1128.78(12) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.088) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 2.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.081) PROFFIT INFO: signal sum: min=-557.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-617.4496 max=1123819.5642 PROFFIT INFO: background sum: min=163.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=405.0000 max=5234.0000 PROFFIT INFO: num of signal pixels: min=37 max=523 PROFFIT INFO: Inet: min=-987.9194 max=1798111.3750 PROFFIT INFO: sig(Inet): min=63.3237 max=24261.9844 PROFFIT INFO: Inet/sig(Inet): min=-1.64 max=202.94 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 448 1804 2674 3198 3428 3980 4316 4524 4854 5064 5120 Percent 8.8 35.2 52.2 62.5 67.0 77.7 84.3 88.4 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2560 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 2560 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1798111- 126913 256 403086.19 76.51 100.00 126173- 4053 256 28518.72 19.75 100.00 4031- 2123 256 2921.25 7.30 98.44 2116- 1227 256 1606.77 3.91 52.34 1225- 816 256 1000.84 2.16 10.94 815- 536 256 669.51 1.65 6.25 535- 317 256 424.55 1.27 6.25 317- 149 256 227.10 0.66 1.17 147- 17 256 76.75 0.27 0.00 17- -988 256 -145.63 -0.28 0.00 ------------------------------------------------------------------------------------ 1798111- -988 2560 43838.60 11.32 37.54 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 256 109376.31 15.04 68.36 1.64- 1.26 256 81239.46 21.24 59.38 1.26- 1.09 256 57851.60 18.54 67.19 1.09- 0.96 256 53420.70 14.45 32.03 0.96- 0.88 256 18129.59 7.42 42.58 0.88- 0.80 256 48431.11 13.55 35.55 0.80- 0.76 256 20106.96 6.15 19.92 0.76- 0.71 256 22340.71 7.20 17.97 0.71- 0.67 256 23597.01 7.69 26.17 0.67- 0.63 256 3892.60 1.93 6.25 ------------------------------------------------------------------------------------ 6.00- 0.63 2560 43838.60 11.32 37.54 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:04:15 2019 Sorting 2560 observations 42 unique observations with > 7.00 F2/sig(F2) 2560 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 49 255 Total number of frames 255 Maximum number of 42 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 2560 observations in 3 runs Run # start # end # total # 1 0 14 15 2 0 14 30 3 0 7 38 Total number of frames 38 618 observations > 7.00 F2/sig(F2) 618 observations in 3 runs Run # start # end # total # 1 0 14 15 2 0 14 30 3 0 6 37 Total number of frames 37 Removing 'redundancy=1' reflections Average redundancy: 13.0 (Out of 618 removed 5 = 613, unique = 47) 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 613 observations in 3 runs Run # start # end # total # 1 0 14 15 2 0 14 30 3 0 6 37 Total number of frames 37 47 unique data precomputed (should be 47) 47 unique data with 613 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 13.0 (Out of 613 removed 0 = 613, unique = 47) 47 unique data precomputed (should be 47) 47 unique data with 613 observations RMS deviation of equivalent data = 0.23238 Rint = 0.18888 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18558, wR= 0.23595 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08034, wR= 0.12379, Acormin=0.604, Acormax=1.314, Acor_av=1.010 F test: Probability=1.000, F= 5.289 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07784, wR= 0.12120, Acormin=0.559, Acormax=1.360, Acor_av=0.978 F test: Probability=0.752, F= 1.060 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06638, wR= 0.10993, Acormin=0.581, Acormax=1.394, Acor_av=0.992 F test: Probability=1.000, F= 1.441 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07004, wR= 0.10792, Acormin=0.556, Acormax=1.411, Acor_av=0.971 F test: Probability=0.000, F= 0.893 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07079, wR= 0.10796, Acormin=0.536, Acormax=1.318, Acor_av=0.922 F test: Probability=0.000, F= 0.863 Final absorption model (ne=4, no=0): Rint= 0.06638, Acormin=0.581, Acormax=1.394, Acor_av=0.992 Combined refinement in use Rint: 0.19101 There are 37 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 0 (14 parameters) Refinement control: 50 pars with 1275 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.23238 Using Levenberg-Marquardt: 0.00010 New wR= 0.11910 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18888 with corrections 0.07787 Rint for all data: 0.19101 with corrections 0.08099 2 observations identified as outliers and rejected Cycle 2 wR= 0.09866 Using Levenberg-Marquardt: 0.00001 New wR= 0.09031 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18595 with corrections 0.06256 Rint for all data: 0.19101 with corrections 0.06987 2 observations identified as outliers and rejected Cycle 3 wR= 0.07901 Using Levenberg-Marquardt: 0.00000 New wR= 0.07375 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18334 with corrections 0.05496 Rint for all data: 0.19101 with corrections 0.06588 0 observations identified as outliers and rejected Cycle 4 wR= 0.07375 Using Levenberg-Marquardt: 0.00000 New wR= 0.07418 Using Levenberg-Marquardt: 0.00000 New wR= 0.07418 Using Levenberg-Marquardt: 0.00001 New wR= 0.07418 Using Levenberg-Marquardt: 0.00010 New wR= 0.07418 Using Levenberg-Marquardt: 0.00100 New wR= 0.07418 Using Levenberg-Marquardt: 0.01000 New wR= 0.07416 Using Levenberg-Marquardt: 0.10000 New wR= 0.07405 Using Levenberg-Marquardt: 1.00000 New wR= 0.07385 Using Levenberg-Marquardt: 10.00000 New wR= 0.07377 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18334 with corrections 0.05489 Rint for all data: 0.19101 with corrections 0.06582 Final wR= 0.07377 Final frame scales: Min= 0.9071 Max= 1.2662 Final absorption correction factors: Amin= 0.5907 Amax= 1.3712 PROFFIT INFO: Inet (after scale3 abspack): min=-941.7153 max=1238358.8750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=59.9888 max=23895.7129 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/103 2560 reflections read from tmp file 120 reflections are rejected (117 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 11 7 4 3 5 5 5 115 Initial Chi^2= 0.55408 Cycle 1, Chi^2= 1.03597 Current error model SIG(F2)^2 = 74.98*I_RAW + 8.77*I_BACK+(0.03592*)^2 Cycle 2, Chi^2= 1.02588 Current error model SIG(F2)^2 = 94.33*I_RAW + 5.18*I_BACK+(0.02866*)^2 Cycle 3, Chi^2= 1.01710 Current error model SIG(F2)^2 = 104.48*I_RAW + 3.55*I_BACK+(0.02601*)^2 Cycle 4, Chi^2= 1.00928 Current error model SIG(F2)^2 = 109.61*I_RAW + 2.84*I_BACK+(0.02508*)^2 Cycle 5, Chi^2= 1.00436 Current error model SIG(F2)^2 = 112.02*I_RAW + 2.54*I_BACK+(0.02475*)^2 Cycle 6, Chi^2= 1.00189 Current error model SIG(F2)^2 = 113.08*I_RAW + 2.42*I_BACK+(0.02462*)^2 Cycle 7, Chi^2= 1.00079 Current error model SIG(F2)^2 = 113.53*I_RAW + 2.37*I_BACK+(0.02456*)^2 Cycle 8, Chi^2= 1.00032 Current error model SIG(F2)^2 = 113.72*I_RAW + 2.34*I_BACK+(0.02454*)^2 Cycle 9, Chi^2= 1.00013 Current error model SIG(F2)^2 = 113.79*I_RAW + 2.34*I_BACK+(0.02453*)^2 Final Chi^2= 1.00013 Final error model SIG(F2)^2 = 113.79*I_RAW + 2.34*I_BACK+(0.02453*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1238359- 123871 256 381923.74 30.70 100.00 122694- 3668 256 29301.39 11.81 100.00 3664- 2072 256 2804.09 5.40 96.48 2072- 1190 256 1554.66 3.56 50.78 1189- 811 256 975.77 2.43 14.06 811- 524 256 662.63 2.16 9.77 521- 318 256 415.60 1.79 7.03 318- 144 256 226.50 1.34 1.56 142- 17 256 75.60 0.73 0.00 17- -942 256 -146.84 -0.58 0.00 ------------------------------------------------------------------------------------ 1238359- -942 2560 41779.31 5.93 37.97 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 256 102183.64 9.80 69.92 1.64- 1.26 256 76283.60 8.93 59.38 1.26- 1.09 256 57773.51 7.92 68.75 1.09- 0.96 256 49605.41 6.33 31.64 0.96- 0.88 256 17828.46 4.60 44.14 0.88- 0.80 256 47000.33 6.90 35.55 0.80- 0.76 256 19315.88 3.77 19.92 0.76- 0.71 256 21077.70 4.60 17.58 0.71- 0.67 256 22912.49 4.78 26.95 0.67- 0.63 256 3812.14 1.69 5.86 ------------------------------------------------------------------------------------ 6.00- 0.63 2560 41779.31 5.93 37.97 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 256 102183.64 9.80 69.92 6.00- 1.26 512 89233.62 9.36 64.65 6.00- 1.09 768 78746.91 8.88 66.02 6.00- 0.96 1024 71461.54 8.25 57.42 6.00- 0.88 1280 60734.92 7.52 54.77 6.00- 0.80 1536 58445.82 7.42 51.56 6.00- 0.76 1792 52855.83 6.90 47.04 6.00- 0.71 2048 48883.56 6.61 43.36 6.00- 0.67 2304 45997.89 6.40 41.54 6.00- 0.63 2560 41779.31 5.93 37.97 ------------------------------------------------------------------------------------ 6.00- 0.63 2560 41779.31 5.93 37.97 Scale applied to data: s=0.807520 (maximum obs:1238358.875,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.066; Rsigma 0.038: data 2560 -> merged 162 With outlier rejection... Rint 0.052; Rsigma 0.038: data 2543 -> merged 162 Rejected total: 17, method kkm 12, method Blessing 5 Completeness direct cell (a, b, c) = (10.412, 10.412, 10.412), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626732, 6.011401 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.38 - 1.76 14 14 16.21 100.00 227 1.74 - 1.27 14 14 18.50 100.00 259 1.26 - 1.06 14 14 20.86 100.00 292 1.05 - 0.97 14 14 17.79 100.00 249 0.95 - 0.88 14 14 19.00 100.00 266 0.87 - 0.81 14 14 16.57 100.00 232 0.80 - 0.76 14 14 17.57 100.00 246 0.76 - 0.72 14 14 14.93 100.00 209 0.72 - 0.69 14 14 15.64 100.00 219 0.69 - 0.65 19 19 13.63 100.00 259 --------------------------------------------------------------- 7.38 - 0.65 145 145 16.95 100.00 2458 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:04:15 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.364215 7.364421 7.379201 120.2659 120.0778 89.7162 2490 Reflections read from file xs2212a.hkl 2490 Reflections used for space-group determination (up to diffraction limit of 0.58A); mean (I/sigma) = 4.66 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1261 1248 1255 1243 1882 1652 1668 2490 N (int>3sigma) = 0 143 149 200 137 246 374 384 559 Mean intensity = 0.0 0.9 0.8 1.2 0.8 1.0 25.0 27.5 26.0 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.4 4.9 4.7 Lattice type: P chosen Volume: 282.21 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 0.0000 -1.0000 Unitcell: 7.342 7.363 7.363 60.01 89.90 60.11 Niggli form: a.a = 53.908 b.b = 54.207 c.c = 54.214 b.c = 27.093 a.c = 0.096 a.b = 26.941 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.377 CUBIC F-lattice R(int) = 0.221 [ 2253] Vol = 1128.8 Cell: 10.407 10.440 10.389 90.00 89.84 89.87 Volume: 1128.84 Matrix: 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.194 RHOMBOHEDRAL R-lattice R(int) = 0.199 [ 1824] Vol = 846.6 Cell: 7.364 7.342 18.065 89.86 90.22 119.92 Volume: 846.63 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 -1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.194 RHOMBOHEDRAL R-lattice R(int) = 0.196 [ 573] Vol = 846.6 Trigonal Cell: 7.364 7.342 18.065 89.86 90.22 119.92 Volume: 846.63 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 -1.0000 2.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.499 ORTHORHOMBIC I-lattice R(int) = 0.171 [ 1811] Vol = 564.4 Cell: 7.364 10.407 7.364 89.79 89.72 90.02 Volume: 564.42 Matrix: 1.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.393 MONOCLINIC I-lattice R(int) = 0.127 [ 1296] Vol = 564.4 Cell: 10.407 7.364 7.364 90.28 90.21 90.02 Volume: 564.42 Matrix:-1.0000 -1.0000 -2.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.097 MONOCLINIC I-lattice R(int) = 0.164 [ 1319] Vol = 564.4 Cell: 7.363 7.342 10.440 89.91 90.09 90.10 Volume: 564.42 Matrix: 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.107 [ 588] Vol = 282.2 Cell: 7.342 7.363 7.363 60.01 89.90 60.11 Volume: 282.21 Matrix: 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 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 1255 0 1660 1654 2490 N (int>3sigma) = 0 0 0 0 200 0 387 387 559 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 26.2 27.0 26.0 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.8 4.7 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.781 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 14 14 182 475 N I>3s 0 0 0 116 0.1 0.1 -0.0 1.7 0.6 0.6 0.1 2.5 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 0.221 2099 Fd-3m 1 1 227 C N N N N 37 2284 0.221 2162 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.407446 10.440480 10.388893 89.9984 89.8373 89.8703 ZERR 1.00 0.010810 0.001012 0.005813 0.0011 0.0006 0.1113 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1114947- 100116 308 297 27 11.0 334567.28 28.79 0.047 0.054 75676- 1748 493 490 27 18.1 5546.93 7.36 0.105 0.118 1652- 752 498 496 27 18.4 1159.36 2.71 0.248 0.303 749- 365 445 444 27 16.4 540.05 1.92 0.367 0.477 356- 75 448 448 27 16.6 231.92 1.16 0.573 0.998 73- -182 368 368 27 13.6 -9.98 0.12 0.977 3.323 ------------------------------------------------------------------------------------------- 1114947- -182 2560 2543 162 15.7 40503.16 5.87 0.052 0.058 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-1.27 489 484 27 17.9 88207.89 9.56 0.042 0.046 0.028 1.26-0.97 518 515 27 19.1 52546.22 6.99 0.045 0.054 0.034 0.97-0.81 526 524 29 18.1 31553.56 5.65 0.061 0.076 0.045 0.80-0.73 444 442 27 16.4 18710.09 3.95 0.061 0.072 0.058 0.72-0.67 385 382 27 14.1 19730.12 4.24 0.091 0.109 0.067 0.66-0.63 198 196 25 7.8 4616.19 1.85 0.151 0.103 0.125 ------------------------------------------------------------------------------------------------------ inf-0.63 2560 2543 162 15.7 40503.16 5.87 0.052 0.058 0.038 inf-0.65 2471 2456 144 17.1 41638.36 5.99 0.051 0.057 0.038 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-1.27 484 27 27 100.0 17.9 88207.89 38.51 0.042 0.010 1.26-0.97 515 27 27 100.0 19.1 52546.22 28.85 0.045 0.010 0.97-0.81 524 29 29 100.0 18.1 31553.56 23.83 0.061 0.013 0.80-0.73 442 27 27 100.0 16.4 18710.09 14.73 0.061 0.017 0.72-0.67 382 27 27 100.0 14.1 19730.12 17.19 0.091 0.019 0.66-0.63 196 25 25 100.0 7.8 4616.19 5.49 0.151 0.050 -------------------------------------------------------------------------------------------- inf-0.63 2543 162 162 100.0 15.7 40503.16 23.65 0.052 0.012 inf-0.65 2456 144 144 100.0 17.1 41638.36 24.30 0.051 0.011 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:11:00 2019) ID: 3668; threads 40; handles 811; mem 515532.00 (1204688.00)kB; time: 1w 4d 23h 21m 48s MEMORY INFO: Memory PF:85.0, Ph:504.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.4,peak PF: 700.2, WS: 471.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:87.0, Ph:505.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.2,peak PF: 700.2, WS: 473.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:11:00 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000098 0.000065 0.000097 ) 0.064809 0.092374 0.027273 ( 0.000112 0.000075 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000133 0.000088 0.000131 ) 7.38096 ( 0.00725 ) 7.36649 ( 0.00766 ) 7.42630 ( 0.00869 ) 120.52449 ( 0.11744 ) 120.40327 ( 0.11416 ) 89.27095 ( 0.08191 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:11:00 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000098 0.000065 0.000097 ) 0.064809 0.092374 0.027273 ( 0.000112 0.000075 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000133 0.000088 0.000131 ) M - matrix: 0.013834 0.004578 0.009193 ( 0.000025 0.000016 0.000022 ) 0.004578 0.014011 0.009364 ( 0.000016 0.000018 0.000018 ) 0.009193 0.009364 0.018517 ( 0.000022 0.000018 0.000035 ) unit cell: 7.381(7) 7.366(8) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | 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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb PROFFITPEAK info: 348 peaks in the peak location table UB fit with 46 obs out of 194 (total:194,skipped:0) (23.71%) UB - matrix: 0.086964 -0.045233 0.015364 ( 0.000202 0.000270 0.000526 ) 0.064669 0.092490 0.027435 ( 0.000161 0.000216 0.000420 ) 0.045515 0.058120 0.132100 ( 0.000177 0.000237 0.000461 ) M - matrix: 0.013816 0.004693 0.009123 ( 0.000044 0.000036 0.000062 ) 0.004693 0.013978 0.009520 ( 0.000036 0.000054 0.000062 ) 0.009123 0.009520 0.018439 ( 0.000062 0.000062 0.000125 ) unit cell: 7.35(2) 7.45(2) 7.44(3) 121.2(4) 119.3(4) 89.9(2) V = 286(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 3, #refl in peak table: 194 #indexed refl 175, indexation with best UB: 90.2062% Lattice: 7.3566 7.3703 7.3850 120.243 119.672 89.984 283.529 Rotation: -23.152 24.183 -35.091 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 180 obs out of 194 (total:194,skipped:0) (92.78%) UB - matrix: 0.087866 -0.044351 0.013175 ( 0.000066 0.000060 0.000087 ) 0.061763 0.094104 0.026079 ( 0.000051 0.000046 0.000066 ) 0.048704 0.055974 0.132955 ( 0.000077 0.000069 0.000101 ) M - matrix: 0.013907 0.004641 0.009244 ( 0.000015 0.000010 0.000014 ) 0.004641 0.013956 0.009312 ( 0.000010 0.000013 0.000013 ) 0.009244 0.009312 0.018531 ( 0.000014 0.000013 0.000027 ) unit cell: 7.357(5) 7.364(5) 7.370(6) 120.15(8) 119.87(8) 89.98(5) V = 282.3(4) OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 UB fit with 180 obs out of 194 (total:194,skipped:0) (92.78%) UB - matrix: 0.087868 -0.044355 0.013176 ( 0.000066 0.000060 0.000087 ) 0.061760 0.094110 0.026078 ( 0.000051 0.000046 0.000066 ) 0.048703 0.055976 0.132955 ( 0.000077 0.000069 0.000101 ) M - matrix: 0.013907 0.004641 0.009244 ( 0.000015 0.000010 0.000014 ) 0.004641 0.013957 0.009312 ( 0.000010 0.000013 0.000013 ) 0.009244 0.009312 0.018531 ( 0.000014 0.000013 0.000027 ) unit cell: 7.357(5) 7.364(5) 7.370(6) 120.15(8) 119.88(8) 89.98(5) V = 282.3(4) OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 194 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Run 3 Omega scan: (-48.000 - 27.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 997 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087868 -0.044355 0.013176 ( 0.000066 0.000060 0.000087 ) 0.061759 0.094111 0.026077 ( 0.000051 0.000046 0.000066 ) 0.048703 0.055976 0.132955 ( 0.000077 0.000069 0.000101 ) M - matrix: 0.013907 0.004641 0.009244 ( 0.000015 0.000010 0.000014 ) 0.004641 0.013958 0.009312 ( 0.000010 0.000013 0.000013 ) 0.009244 0.009312 0.018531 ( 0.000014 0.000013 0.000027 ) UB fit with 180 obs out of 194 (total:194,skipped:0) (92.78%) unit cell: 7.357(5) 7.364(5) 7.370(6) 120.15(8) 119.88(8) 89.98(5) V = 282.3(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 180 obs out of 194 (total:194,skipped:0) (92.78%) 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! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb 0 of 172 peaks identified as outliers and rejected 172 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 172 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 172 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.36 | 17 | 0.858 ( 0.098) | 0.866 ( 0.139) | 1.105 ( 0.532) | 2.36- 1.75 | 17 | 0.891 ( 0.105) | 0.898 ( 0.154) | 1.058 ( 0.536) | 1.75- 1.58 | 17 | 0.912 ( 0.079) | 0.953 ( 0.118) | 0.741 ( 0.190) | 1.58- 1.35 | 17 | 0.964 ( 0.070) | 0.994 ( 0.114) | 0.927 ( 0.428) | 1.35- 1.19 | 17 | 0.953 ( 0.075) | 0.958 ( 0.140) | 0.928 ( 0.474) | 1.19- 1.06 | 17 | 0.976 ( 0.072) | 1.005 ( 0.132) | 0.889 ( 0.424) | 1.06- 0.89 | 17 | 0.991 ( 0.055) | 1.005 ( 0.108) | 1.081 ( 0.407) | 0.89- 0.82 | 17 | 0.990 ( 0.058) | 0.991 ( 0.126) | 0.963 ( 0.442) | 0.82- 0.72 | 17 | 0.999 ( 0.048) | 1.008 ( 0.126) | 1.099 ( 0.402) | 0.72- 0.63 | 19 | 0.975 ( 0.055) | 0.894 ( 0.115) | 1.264 ( 0.551) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.63 | 172 | 0.951 ( 0.086) | 0.957 ( 0.137) | 1.008 ( 0.472) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 172 obs out of 172 (total:172,skipped:0) (100.00%) UB - matrix: 0.087983 -0.044352 0.013130 ( 0.000038 0.000036 0.000049 ) 0.061831 0.094112 0.026112 ( 0.000025 0.000023 0.000033 ) 0.048751 0.055785 0.133143 ( 0.000039 0.000036 0.000050 ) M - matrix: 0.013941 0.004636 0.009261 ( 0.000008 0.000005 0.000007 ) 0.004636 0.013936 0.009303 ( 0.000005 0.000007 0.000007 ) 0.009261 0.009303 0.018581 ( 0.000007 0.000007 0.000014 ) unit cell: 7.345(3) 7.363(2) 7.353(3) 120.09(4) 119.86(4) 90.00(3) V = 281.43(19) OTKP changes: 172 1 1 1 OTKP changes: 172 1 1 1 UB - matrix: 0.087813 -0.044297 0.013200 ( 0.000036 0.000034 0.000047 ) 0.061854 0.094021 0.026138 ( 0.000026 0.000024 0.000034 ) 0.048728 0.055850 0.132980 ( 0.000031 0.000029 0.000040 ) M - matrix: 0.013912 0.004647 0.009256 ( 0.000008 0.000005 0.000007 ) 0.004647 0.013921 0.009300 ( 0.000005 0.000006 0.000006 ) 0.009256 0.009300 0.018541 ( 0.000007 0.000006 0.000011 ) UB fit with 172 obs out of 172 (total:172,skipped:0) (100.00%) unit cell: 7.359(3) 7.372(2) 7.368(3) 120.11(4) 119.89(4) 90.03(3) V = 282.59(17) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 27.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.052) HKL list info: 997 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087813 -0.044297 0.013200 ( 0.000036 0.000034 0.000047 ) 0.061854 0.094021 0.026138 ( 0.000026 0.000024 0.000034 ) 0.048728 0.055850 0.132980 ( 0.000031 0.000029 0.000040 ) M - matrix: 0.013912 0.004647 0.009256 ( 0.000008 0.000005 0.000007 ) 0.004647 0.013921 0.009300 ( 0.000005 0.000006 0.000006 ) 0.009256 0.009300 0.018541 ( 0.000007 0.000006 0.000011 ) UB fit with 172 obs out of 172 (total:172,skipped:0) (100.00%) unit cell: 7.359(3) 7.372(2) 7.368(3) 120.11(4) 119.89(4) 90.03(3) V = 282.59(17) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 172 obs out of 172 (total:172,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb 0 of 172 peaks identified as outliers and rejected 172 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 172 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 172 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 17 | 0.870 ( 0.092) | 0.882 ( 0.122) | 1.086 ( 0.564) | 2.37- 1.76 | 17 | 0.879 ( 0.114) | 0.884 ( 0.173) | 1.050 ( 0.581) | 1.75- 1.58 | 17 | 0.919 ( 0.080) | 0.968 ( 0.107) | 0.732 ( 0.201) | 1.58- 1.36 | 17 | 0.941 ( 0.088) | 0.967 ( 0.129) | 0.859 ( 0.447) | 1.35- 1.20 | 17 | 0.952 ( 0.075) | 0.959 ( 0.138) | 0.931 ( 0.490) | 1.20- 1.06 | 17 | 0.974 ( 0.066) | 0.993 ( 0.134) | 0.882 ( 0.413) | 1.06- 0.91 | 17 | 0.996 ( 0.056) | 1.008 ( 0.111) | 1.094 ( 0.407) | 0.89- 0.82 | 17 | 0.992 ( 0.057) | 0.981 ( 0.104) | 1.051 ( 0.482) | 0.82- 0.72 | 17 | 0.997 ( 0.051) | 0.987 ( 0.118) | 1.180 ( 0.502) | 0.72- 0.63 | 19 | 0.978 ( 0.054) | 0.923 ( 0.142) | 1.182 ( 0.489) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 172 | 0.950 ( 0.088) | 0.955 ( 0.136) | 1.007 ( 0.489) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.6 | 64 | 0.977 ( 0.040) | 1.020 ( 0.084) | 1.158 ( 0.501) | 10.7-14.9 | 64 | 0.983 ( 0.043) | 1.042 ( 0.061) | 1.185 ( 0.548) | 15.0-19.3 | 64 | 0.994 ( 0.260) | 1.020 ( 0.108) | 1.232 ( 1.320) | 19.4-23.5 | 64 | 0.956 ( 0.057) | 1.001 ( 0.084) | 0.946 ( 0.421) | 23.5-27.1 | 64 | 0.957 ( 0.062) | 0.990 ( 0.096) | 0.973 ( 0.451) | 27.2-32.6 | 64 | 0.939 ( 0.091) | 0.943 ( 0.116) | 0.934 ( 0.470) | 32.7-36.4 | 64 | 0.923 ( 0.187) | 0.906 ( 0.134) | 1.086 ( 0.711) | 36.5-39.0 | 64 | 0.878 ( 0.092) | 0.844 ( 0.124) | 0.986 ( 0.494) | 39.0-42.0 | 64 | 0.889 ( 0.095) | 0.833 ( 0.127) | 1.097 ( 0.492) | 42.0-50.1 | 62 | 0.869 ( 0.114) | 0.793 ( 0.131) | 0.971 ( 0.495) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 638 | 0.937 ( 0.130) | 0.939 ( 0.138) | 1.057 ( 0.651) | Fitted profile normalization line parameters e1 dimension: a=-0.0035 b=1.14 e2 dimension: a=-0.0073 b=1.25 e3 dimension: a=0.0019 b=1.03 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:11:10 2019 PROFFITMAIN - Started at Wed Aug 21 13:11:10 2019 OTKP changes: 293 2 2 3 OTKP changes: 293 2 2 3 OTKP changes: 293 2 2 3 UB - matrix: 0.087620 -0.046059 0.016870 ( 0.000092 0.000063 0.000091 ) 0.063718 0.092455 0.026990 ( 0.000102 0.000070 0.000102 ) 0.045483 0.057721 0.132175 ( 0.000108 0.000074 0.000108 ) M - matrix: 0.013806 0.004481 0.009210 ( 0.000023 0.000014 0.000019 ) 0.004481 0.014001 0.009348 ( 0.000014 0.000017 0.000016 ) 0.009210 0.009348 0.018483 ( 0.000019 0.000016 0.000029 ) UB fit with 337 obs out of 638 (total:638,skipped:0) (52.82%) unit cell: 7.389(7) 7.367(7) 7.428(7) 120.73(10) 120.35(10) 88.90(8) V = 284.0(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 203 obs out of 212 (total:212,skipped:0) (95.75%) UB - matrix: 0.087557 -0.046201 0.017205 ( 0.000109 0.000068 0.000101 ) 0.064769 0.092387 0.027146 ( 0.000088 0.000054 0.000081 ) 0.045949 0.057790 0.132152 ( 0.000105 0.000066 0.000098 ) M - matrix: 0.013973 0.004594 0.009337 ( 0.000024 0.000014 0.000018 ) 0.004594 0.014009 0.009350 ( 0.000014 0.000014 0.000014 ) 0.009337 0.009350 0.018497 ( 0.000018 0.000014 0.000026 ) unit cell: 7.372(7) 7.362(6) 7.435(6) 120.49(9) 120.49(10) 89.22(7) V = 283.0(4) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.106) HKL list info: 1285 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087480 -0.046160 0.017361 ( 0.000099 0.000062 0.000092 ) 0.064780 0.092379 0.027251 ( 0.000086 0.000053 0.000080 ) 0.045706 0.057853 0.132160 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013938 0.004590 0.009325 ( 0.000023 0.000013 0.000018 ) 0.004590 0.014011 0.009362 ( 0.000013 0.000014 0.000013 ) 0.009325 0.009362 0.018510 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.379(6) 7.365(6) 7.433(6) 120.53(9) 120.46(9) 89.22(7) V = 283.3(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118065 0.039058 0.078744 ( 0.000074 0.000046 0.000068 ) 0.000077 0.111604 0.056285 ( 0.000078 0.000049 0.000072 ) -0.000055 -0.000060 0.095456 ( 0.000089 0.000055 0.000082 ) M - matrix: 0.013939 0.004620 0.009296 ( 0.000017 0.000011 0.000014 ) 0.004620 0.013981 0.009351 ( 0.000011 0.000011 0.000011 ) 0.009296 0.009351 0.018480 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.370(5) 7.376(5) 7.426(8) 120.47(9) 120.25(9) 89.48(6) V = 283.6(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 172 obs out of 172 (total:172,skipped:0) (100.00%) UB - matrix: 0.087811 -0.044299 0.013187 ( 0.000036 0.000034 0.000047 ) 0.061855 0.094027 0.026138 ( 0.000026 0.000025 0.000034 ) 0.048726 0.055836 0.132983 ( 0.000031 0.000029 0.000040 ) M - matrix: 0.013911 0.004647 0.009254 ( 0.000008 0.000005 0.000006 ) 0.004647 0.013921 0.009299 ( 0.000005 0.000006 0.000006 ) 0.009254 0.009299 0.018541 ( 0.000006 0.000006 0.000011 ) unit cell: 7.358(3) 7.372(2) 7.367(2) 120.10(4) 119.88(4) 90.03(3) V = 282.56(17) OTKP changes: 172 1 1 1 OTKP changes: 172 1 1 1 OTKP changes: 172 1 1 1 UB - matrix: 0.087815 -0.044295 0.013193 ( 0.000036 0.000034 0.000046 ) 0.061860 0.094028 0.026131 ( 0.000026 0.000025 0.000034 ) 0.048733 0.055841 0.132987 ( 0.000031 0.000029 0.000040 ) M - matrix: 0.013913 0.004648 0.009256 ( 0.000008 0.000005 0.000006 ) 0.004648 0.013921 0.009299 ( 0.000005 0.000006 0.000006 ) 0.009256 0.009299 0.018542 ( 0.000006 0.000006 0.000011 ) UB fit with 172 obs out of 172 (total:172,skipped:0) (100.00%) unit cell: 7.358(3) 7.372(2) 7.367(2) 120.10(4) 119.88(4) 90.04(3) V = 282.53(17) Run 3 Omega scan: (-48.000 - 27.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.052) HKL list info: 979 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087815 -0.044295 0.013193 ( 0.000036 0.000034 0.000046 ) 0.061860 0.094028 0.026131 ( 0.000026 0.000025 0.000034 ) 0.048733 0.055841 0.132987 ( 0.000031 0.000029 0.000040 ) M - matrix: 0.013913 0.004648 0.009256 ( 0.000008 0.000005 0.000006 ) 0.004648 0.013921 0.009299 ( 0.000005 0.000006 0.000006 ) 0.009256 0.009299 0.018542 ( 0.000006 0.000006 0.000011 ) UB fit with 172 obs out of 172 (total:172,skipped:0) (100.00%) unit cell: 7.358(3) 7.372(2) 7.367(2) 120.10(4) 119.88(4) 90.04(3) V = 282.53(17) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 172 obs out of 172 (total:172,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: 0.087815 -0.044295 0.013193 ( 0.000036 0.000034 0.000046 ) 0.061860 0.094028 0.026131 ( 0.000026 0.000025 0.000034 ) 0.048733 0.055841 0.132987 ( 0.000031 0.000029 0.000040 ) M - matrix: 0.013913 0.004648 0.009256 ( 0.000008 0.000005 0.000006 ) 0.004648 0.013921 0.009299 ( 0.000005 0.000006 0.000006 ) 0.009256 0.009299 0.018542 ( 0.000006 0.000006 0.000011 ) UB fit with 172 obs out of 172 (total:172,skipped:0) (100.00%) unit cell: 7.358(3) 7.372(2) 7.367(2) 120.10(4) 119.88(4) 90.04(3) V = 282.53(17) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117951 0.039081 0.078673 ( 0.000030 0.000030 0.000036 ) 0.000080 0.111517 0.056199 ( 0.000029 0.000028 0.000034 ) -0.000054 -0.000133 0.096067 ( 0.000033 0.000032 0.000039 ) M - matrix: 0.013912 0.004619 0.009279 ( 0.000007 0.000005 0.000006 ) 0.004619 0.013963 0.009329 ( 0.000005 0.000007 0.000006 ) 0.009279 0.009329 0.018577 ( 0.000006 0.000006 0.000010 ) UB fit with 632 obs out of 638 (total:638,skipped:0) (99.06%) unit cell: 7.364(2) 7.364(2) 7.376(3) 120.24(4) 120.06(4) 89.75(3) V = 282.20(17) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 72 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof 2814 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:11:15 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.106) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 27.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.052) PROFFIT INFO: signal sum: min=-564.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-613.1116 max=1115393.0011 PROFFIT INFO: background sum: min=163.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=441.0000 max=5104.0000 PROFFIT INFO: num of signal pixels: min=42 max=510 PROFFIT INFO: Inet: min=-980.9785 max=1784628.8750 PROFFIT INFO: sig(Inet): min=63.1934 max=24344.3242 PROFFIT INFO: Inet/sig(Inet): min=-1.69 max=199.51 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 250 970 1465 1751 1883 2188 2375 2483 2670 2784 2814 Percent 8.9 34.5 52.1 62.2 66.9 77.8 84.4 88.2 94.9 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2814 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 2814 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1784629- 129278 281 407377.93 76.37 100.00 128866- 4011 281 28734.83 19.63 100.00 3975- 2130 281 2928.03 7.34 98.93 2119- 1245 281 1621.28 3.85 53.02 1243- 829 281 1013.55 2.18 11.39 828- 553 281 683.50 1.69 7.47 550- 327 281 437.30 1.28 6.41 326- 159 281 239.79 0.69 1.07 158- 17 281 80.87 0.28 0.00 17- -981 285 -142.74 -0.27 0.00 ------------------------------------------------------------------------------------ 1784629- -981 2814 44234.26 11.29 37.78 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 281 102363.68 17.48 69.04 1.59- 1.22 281 85603.58 18.68 57.65 1.22- 1.02 281 62832.85 17.27 52.67 1.02- 0.90 281 33499.14 10.13 38.43 0.90- 0.81 281 28071.96 9.16 33.45 0.81- 0.74 281 41043.94 12.16 39.50 0.74- 0.68 281 28175.60 8.58 25.27 0.68- 0.62 281 26053.54 7.92 24.20 0.62- 0.57 281 17658.41 5.99 20.64 0.57- 0.45 285 17421.64 5.60 17.19 ------------------------------------------------------------------------------------ 6.55- 0.45 2814 44234.26 11.29 37.78 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:11:15 2019 Sorting 2814 observations 83 unique observations with > 7.00 F2/sig(F2) 2814 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 74 280 Total number of frames 280 Maximum number of 83 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 2814 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 18 71 Total number of frames 71 679 observations > 7.00 F2/sig(F2) 679 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 18 71 Total number of frames 71 Removing 'redundancy=1' reflections Average redundancy: 5.6 (Out of 679 removed 40 = 639, unique = 115) 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 639 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 18 71 Total number of frames 71 115 unique data precomputed (should be 115) 115 unique data with 639 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.6 (Out of 639 removed 0 = 639, unique = 115) 115 unique data precomputed (should be 115) 115 unique data with 639 observations RMS deviation of equivalent data = 0.38812 Rint = 0.35149 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.34860, wR= 0.46328 Trying model 1 (ne=2, no=0)... Results: Rint= 0.24836, wR= 0.33648, Acormin=0.507, Acormax=1.539, Acor_av=0.977 F test: Probability=1.000, F= 1.951 Trying model 2 (ne=2, no=1)... Results: Rint= 0.25612, wR= 0.34454, Acormin=0.284, Acormax=1.596, Acor_av=0.867 F test: Probability=0.000, F= 0.935 Trying model 3 (ne=4, no=0)... Results: Rint= 0.24938, wR= 0.32833, Acormin=0.493, Acormax=1.633, Acor_av=0.947 F test: Probability=0.000, F= 0.975 Trying model 4 (ne=4, no=1)... Results: Rint= 0.25711, wR= 0.34014, Acormin=0.261, Acormax=1.706, Acor_av=0.858 F test: Probability=0.000, F= 0.911 Trying model 5 (ne=4, no=3)... Results: Rint= 0.25700, wR= 0.32982, Acormin=0.194, Acormax=1.583, Acor_av=0.777 F test: Probability=0.000, F= 0.900 Trying model 6 (ne=6, no=0)... Results: Rint= 0.25307, wR= 0.30449, Acormin=0.176, Acormax=1.751, Acor_av=0.830 F test: Probability=0.000, F= 0.922 Trying model 7 (ne=6, no=1)... Results: Rint= 0.25879, wR= 0.30705, Acormin=0.028, Acormax=1.796, Acor_av=0.804 F test: Probability=0.000, F= 0.877 Trying model 8 (ne=6, no=3)... Results: Rint= 0.25815, wR= 0.30330, Acormin=0.005, Acormax=1.652, Acor_av=0.722 F test: Probability=0.000, F= 0.868 Trying model 9 (ne=6, no=5)... Results: Rint= 0.28968, wR= 0.31882, Acormin=-0.039, Acormax=1.400, Acor_av=0.393 F test: Probability=0.000, F= 0.674 Trying model 10 (ne=8, no=0)... Results: Rint= 0.25608, wR= 0.30333, Acormin=0.046, Acormax=2.186, Acor_av=0.710 F test: Probability=0.000, F= 0.870 Trying model 11 (ne=8, no=1)... Results: Rint= 0.34014, wR= 0.38444, Acormin=-0.128, Acormax=1.448, Acor_av=0.427 F test: Probability=0.000, F= 0.490 Trying model 12 (ne=8, no=3)... Results: Rint= 0.29095, wR= 0.32496, Acormin=-0.010, Acormax=0.096, Acor_av=0.046 F test: Probability=0.000, F= 0.660 Trying model 13 (ne=8, no=5)... Results: Rint= 0.22775, wR= 0.25601, Acormin=-0.001, Acormax=0.138, Acor_av=0.057 F test: Probability=0.709, F= 1.051 Trying model 14 (ne=8, no=7)... Results: Rint= 0.15780, wR= 0.20183, Acormin=0.011, Acormax=0.158, Acor_av=0.060 F test: Probability=1.000, F= 2.119 Final absorption model (ne=2, no=0): Rint= 0.24836, Acormin=0.507, Acormax=1.539, Acor_av=0.977 Combined refinement in use Rint: 0.36601 There are 71 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 75 pars with 2850 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.38812 Using Levenberg-Marquardt: 0.00010 New wR= 0.21553 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35149 with corrections 0.18948 Rint for all data: 0.36601 with corrections 0.20589 0 observations identified as outliers and rejected Cycle 2 wR= 0.21553 Using Levenberg-Marquardt: 0.00001 New wR= 0.20841 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35149 with corrections 0.18241 Rint for all data: 0.36601 with corrections 0.19888 0 observations identified as outliers and rejected Cycle 3 wR= 0.20841 Using Levenberg-Marquardt: 0.00000 New wR= 0.20540 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35149 with corrections 0.18282 Rint for all data: 0.36601 with corrections 0.19926 0 observations identified as outliers and rejected Cycle 4 wR= 0.20540 Using Levenberg-Marquardt: 0.00000 New wR= 0.20605 Using Levenberg-Marquardt: 0.00000 New wR= 0.20605 Using Levenberg-Marquardt: 0.00001 New wR= 0.20605 Using Levenberg-Marquardt: 0.00010 New wR= 0.20605 Using Levenberg-Marquardt: 0.00100 New wR= 0.20599 Using Levenberg-Marquardt: 0.01000 New wR= 0.20567 Using Levenberg-Marquardt: 0.10000 New wR= 0.20534 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35149 with corrections 0.18220 Rint for all data: 0.36601 with corrections 0.19863 Final wR= 0.20534 Final frame scales: Min= 0.5257 Max= 1.9086 Final absorption correction factors: Amin= 0.5122 Amax= 1.4971 PROFFIT INFO: Inet (after scale3 abspack): min=-1861.3495 max=1546778.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=44.6535 max=26998.4121 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/103 2814 reflections read from tmp file 751 reflections are rejected (670 as outliers, 81 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 76 70 42 42 27 31 22 17 53 Initial Chi^2= 2.49605 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.79393 Current error model SIG(F2)^2 = 545.93*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 433.43*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 433.43*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1546778- 114706 281 373175.23 31.47 100.00 114023- 4004 281 25337.66 6.67 81.14 4001- 2013 281 2676.84 2.65 29.89 2011- 1155 281 1550.30 1.95 15.66 1149- 748 281 923.65 1.35 2.14 746- 488 281 609.24 1.13 0.36 485- 301 281 388.02 0.99 0.36 300- 141 281 220.85 0.82 0.00 140- 15 281 73.42 0.47 0.00 15- -1861 285 -166.30 -0.34 0.00 ------------------------------------------------------------------------------------ 1546778- -1861 2814 40421.12 4.71 22.92 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 281 103047.06 10.88 52.67 1.59- 1.22 281 80170.04 8.27 39.86 1.22- 1.02 281 61246.79 6.62 32.38 1.02- 0.90 281 30705.33 3.64 16.73 0.90- 0.81 281 25001.88 3.31 14.59 0.81- 0.74 281 36131.27 4.19 21.35 0.74- 0.68 281 23535.33 3.08 12.46 0.68- 0.62 281 20486.35 2.84 13.88 0.62- 0.57 281 13403.54 2.24 13.17 0.57- 0.45 285 10903.75 2.07 12.28 ------------------------------------------------------------------------------------ 6.55- 0.45 2814 40421.12 4.71 22.92 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 281 103047.06 10.88 52.67 6.55- 1.22 562 91608.55 9.57 46.26 6.55- 1.02 843 81487.96 8.59 41.64 6.55- 0.90 1124 68792.30 7.35 35.41 6.55- 0.81 1405 60034.22 6.54 31.25 6.55- 0.74 1686 56050.39 6.15 29.60 6.55- 0.68 1967 51405.39 5.71 27.15 6.55- 0.62 2248 47540.51 5.35 25.49 6.55- 0.57 2529 43747.51 5.01 24.12 6.55- 0.45 2814 40421.12 4.71 22.92 ------------------------------------------------------------------------------------ 6.55- 0.45 2814 40421.12 4.71 22.92 Scale applied to data: s=0.646504 (maximum obs:1546778.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.199; Rsigma 0.051: data 2814 -> merged 466 With outlier rejection... Rint 0.178; Rsigma 0.053: data 2737 -> merged 466 Rejected total: 77, method kkm 70, method Blessing 7 Completeness direct cell (a, b, c) = (6.559, 6.559, 6.559), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.449430, 6.559215 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.59 22 22 13.68 100.00 301 1.55 - 1.22 22 22 12.91 100.00 284 1.20 - 1.02 22 22 11.45 100.00 252 1.02 - 0.92 22 22 10.00 100.00 220 0.92 - 0.84 22 22 9.55 100.00 210 0.84 - 0.79 22 22 7.73 100.00 170 0.79 - 0.75 22 22 8.14 100.00 179 0.75 - 0.71 22 22 6.36 100.00 140 0.71 - 0.69 22 22 6.68 100.00 147 0.68 - 0.65 26 29 6.04 89.66 157 --------------------------------------------------------------- 7.37 - 0.65 224 227 9.20 98.68 2060 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:11:16 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.364025 7.363737 7.376201 120.2355 120.0592 89.7455 2737 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.39 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1390 1384 1384 1378 2079 1824 1824 2737 N (int>3sigma) = 0 154 157 217 153 264 403 411 599 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 21.7 24.0 23.4 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.1 4.6 4.4 Lattice type: P chosen Volume: 282.20 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.344 7.364 7.364 120.00 119.80 90.10 Niggli form: a.a = 53.930 b.b = 54.221 c.c = 54.225 b.c = -27.110 a.c = -26.873 a.b = -0.090 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.315 CUBIC F-lattice R(int) = 0.238 [ 2500] Vol = 1128.8 Cell: 10.437 10.408 10.391 89.85 90.00 89.90 Volume: 1128.80 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.458 TETRAGONAL I-lattice R(int) = 0.222 [ 2123] Vol = 564.4 Cell: 7.364 7.376 10.391 90.11 89.89 89.84 Volume: 564.40 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.350 TETRAGONAL I-lattice R(int) = 0.208 [ 2117] Vol = 564.4 Cell: 7.344 7.364 10.437 90.07 89.93 90.10 Volume: 564.40 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.124 TETRAGONAL I-lattice R(int) = 0.222 [ 2123] Vol = 564.4 Cell: 7.376 7.364 10.391 90.11 90.11 90.16 Volume: 564.40 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.415 ORTHORHOMBIC F-lattice R(int) = 0.181 [ 2084] Vol = 1128.8 Cell: 10.391 10.408 10.437 89.90 90.00 89.85 Volume: 1128.80 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.452 ORTHORHOMBIC I-lattice R(int) = 0.172 [ 2053] Vol = 564.4 Cell: 10.391 7.376 7.364 89.84 89.89 90.11 Volume: 564.40 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.129 ORTHORHOMBIC I-lattice R(int) = 0.211 [ 2056] Vol = 564.4 Cell: 7.344 7.364 10.437 89.93 90.07 90.10 Volume: 564.40 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.309 MONOCLINIC I-lattice R(int) = 0.112 [ 1586] Vol = 564.4 Cell: 7.364 10.391 7.376 90.11 90.16 90.11 Volume: 564.40 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.342 MONOCLINIC I-lattice R(int) = 0.177 [ 1580] Vol = 564.4 Cell: 7.364 10.408 7.364 89.96 90.25 89.82 Volume: 564.40 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.308 MONOCLINIC I-lattice R(int) = 0.112 [ 1586] Vol = 564.4 Cell: 7.376 10.391 7.364 90.11 90.16 90.11 Volume: 564.40 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.090 MONOCLINIC I-lattice R(int) = 0.189 [ 1544] Vol = 564.4 Cell: 7.344 7.364 10.437 90.07 90.07 89.90 Volume: 564.40 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.065 MONOCLINIC I-lattice R(int) = 0.177 [ 1582] Vol = 564.4 Cell: 7.344 10.437 7.364 90.07 90.10 89.93 Volume: 564.40 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.093 MONOCLINIC I-lattice R(int) = 0.177 [ 1582] Vol = 564.4 Cell: 7.344 10.437 7.364 89.93 90.10 90.07 Volume: 564.40 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.111 [ 696] Vol = 282.2 Cell: 7.344 7.364 7.364 120.00 119.80 90.10 Volume: 282.20 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 1384 0 1817 1817 2737 N (int>3sigma) = 0 0 0 0 217 0 417 411 599 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 24.3 22.8 23.4 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.5 4.4 4.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.787 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 16 16 206 530 N I>3s 0 0 0 126 0.0 0.0 -0.0 1.6 0.5 0.5 0.1 2.5 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 0.238 2322 Fd-3m 1 1 227 C N N N N 37 2284 0.237 2385 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.437204 10.408261 10.390946 89.8457 90.0022 89.9034 ZERR 1.00 0.000982 0.010495 0.005676 0.0000 0.0001 0.1064 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 988570- 100769 301 269 46 5.8 343684.33 29.62 0.158 0.140 100342- 2776 327 313 46 6.8 14366.48 4.61 0.303 0.160 2765- 1541 478 470 46 10.2 2099.10 2.15 0.853 0.949 1540- 1014 415 406 46 8.8 1171.08 1.39 0.765 0.832 1011- 776 306 303 46 6.6 872.19 1.16 0.680 0.722 765- 562 274 270 46 5.9 649.31 0.96 0.666 0.718 562- 448 228 225 46 4.9 479.72 0.80 0.687 0.825 445- 310 186 184 46 4.0 371.52 0.76 0.675 0.763 308- 140 170 169 46 3.7 219.27 0.51 0.811 1.214 137- -696 129 128 52 2.5 39.36 0.18 0.967 2.183 ------------------------------------------------------------------------------------------- 988570- -696 2814 2737 466 5.9 36195.76 4.39 0.178 0.154 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-1.20 632 614 46 13.3 68927.69 7.93 0.181 0.146 0.029 1.16-0.90 511 496 49 10.1 47752.18 5.15 0.186 0.169 0.050 0.89-0.77 406 396 46 8.6 34905.51 4.09 0.173 0.164 0.069 0.77-0.70 351 344 49 7.0 25529.17 3.38 0.181 0.184 0.077 0.69-0.64 292 279 48 5.8 14929.09 2.24 0.150 0.134 0.104 0.63-0.59 225 220 48 4.6 11864.16 2.11 0.163 0.155 0.125 0.59-0.56 157 151 48 3.1 10857.69 1.94 0.163 0.148 0.121 0.55-0.53 106 103 46 2.2 9725.52 1.97 0.115 0.112 0.129 0.52-0.49 83 83 46 1.8 8355.71 1.82 0.056 0.053 0.130 0.49-0.45 51 51 40 1.3 6792.38 1.62 0.067 0.068 0.137 ------------------------------------------------------------------------------------------------------ inf-0.45 2814 2737 466 5.9 36195.76 4.39 0.178 0.154 0.053 inf-0.65 2122 2060 224 9.2 43771.74 5.10 0.180 0.157 0.047 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-1.20 614 46 46 100.0 13.3 68927.69 25.79 0.181 0.011 1.16-0.90 496 49 49 100.0 10.1 47752.18 14.50 0.186 0.022 0.89-0.77 396 46 46 100.0 8.6 34905.51 11.62 0.173 0.033 0.77-0.70 344 49 49 100.0 7.0 25529.17 8.83 0.181 0.033 0.69-0.64 279 51 48 94.1 5.8 14929.09 5.30 0.150 0.054 0.63-0.59 220 51 48 94.1 4.6 11864.16 4.18 0.163 0.069 0.59-0.56 151 57 48 84.2 3.1 10857.69 3.41 0.163 0.070 0.55-0.53 103 61 46 75.4 2.2 9725.52 2.87 0.115 0.079 0.52-0.49 83 84 46 54.8 1.8 8355.71 2.45 0.056 0.092 0.49-0.45 51 145 40 27.6 1.3 6792.38 1.96 0.067 0.098 -------------------------------------------------------------------------------------------- inf-0.45 2737 640 466 72.8 5.9 36195.76 12.49 0.178 0.030 inf-0.65 2060 227 224 98.7 9.2 43771.74 15.23 0.180 0.021 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 No constraint UB - matrix: 0.012756 -0.008706 -0.066460 ( 0.000014 0.000015 0.000013 ) 0.065178 -0.013294 0.014304 ( 0.000014 0.000015 0.000013 ) -0.014609 -0.066269 0.006007 ( 0.000018 0.000018 0.000016 ) M - matrix: 0.004624 -0.000009 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000009 0.004644 -0.000010 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000010 0.004658 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.012756 -0.008706 -0.066460 ( 0.000014 0.000015 0.000013 ) 0.065178 -0.013294 0.014304 ( 0.000014 0.000015 0.000013 ) -0.014609 -0.066269 0.006007 ( 0.000018 0.000018 0.000016 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) unit cell: 10.431(2) 10.408(2) 10.393(2) 89.881(18) 89.960(18) 89.883(19) V = 1128.3(4) unit cell: 10.4106(6) 10.4106(6) 10.4106(6) 90.0 90.0 90.0 V = 1128.32(11) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.106) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 27.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.052) PROFFIT INFO: signal sum: min=-564.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-613.1116 max=1115393.0011 PROFFIT INFO: background sum: min=163.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=441.0000 max=5104.0000 PROFFIT INFO: num of signal pixels: min=42 max=510 PROFFIT INFO: Inet: min=-980.9785 max=1784628.8750 PROFFIT INFO: sig(Inet): min=63.1934 max=24344.3242 PROFFIT INFO: Inet/sig(Inet): min=-1.69 max=199.51 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 500 1940 2930 3502 3766 4376 4750 4966 5340 5568 5628 Percent 8.9 34.5 52.1 62.2 66.9 77.8 84.4 88.2 94.9 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2814 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 2814 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1784629- 129278 281 407377.93 76.37 100.00 128866- 4011 281 28734.83 19.63 100.00 3975- 2130 281 2928.03 7.34 98.93 2119- 1245 281 1621.28 3.85 53.02 1243- 829 281 1013.55 2.18 11.39 828- 553 281 683.50 1.69 7.47 550- 327 281 437.30 1.28 6.41 326- 159 281 239.79 0.69 1.07 158- 17 281 80.87 0.28 0.00 17- -981 285 -142.74 -0.27 0.00 ------------------------------------------------------------------------------------ 1784629- -981 2814 44234.26 11.29 37.78 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 281 108736.68 14.69 68.33 1.64- 1.26 281 85650.15 21.63 59.79 1.26- 1.09 281 56664.12 17.95 66.90 1.09- 0.96 281 53014.11 14.29 32.74 0.96- 0.88 281 17364.85 7.22 43.42 0.88- 0.81 281 51536.09 14.29 37.01 0.81- 0.76 281 19220.03 5.96 19.22 0.76- 0.71 281 23796.70 7.56 18.51 0.71- 0.67 281 23004.52 7.54 26.33 0.67- 0.63 285 3929.15 1.90 5.96 ------------------------------------------------------------------------------------ 6.00- 0.63 2814 44234.26 11.29 37.78 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:11:16 2019 Sorting 2814 observations 43 unique observations with > 7.00 F2/sig(F2) 2814 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 74 280 Total number of frames 280 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 2814 observations in 3 runs Run # start # end # total # 1 0 14 15 2 0 14 30 3 0 10 41 Total number of frames 41 679 observations > 7.00 F2/sig(F2) 679 observations in 3 runs Run # start # end # total # 1 0 14 15 2 0 14 30 3 0 10 41 Total number of frames 41 Removing 'redundancy=1' reflections Average redundancy: 13.5 (Out of 679 removed 2 = 677, unique = 50) 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 677 observations in 3 runs Run # start # end # total # 1 0 14 15 2 0 14 30 3 0 10 41 Total number of frames 41 50 unique data precomputed (should be 50) 50 unique data with 677 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 13.5 (Out of 677 removed 0 = 677, unique = 50) 50 unique data precomputed (should be 50) 50 unique data with 677 observations RMS deviation of equivalent data = 0.23464 Rint = 0.18383 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17987, wR= 0.23487 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07815, wR= 0.12281, Acormin=0.609, Acormax=1.314, Acor_av=0.991 F test: Probability=1.000, F= 5.256 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07618, wR= 0.11893, Acormin=0.555, Acormax=1.357, Acor_av=0.966 F test: Probability=0.717, F= 1.047 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06596, wR= 0.10781, Acormin=0.587, Acormax=1.400, Acor_av=0.979 F test: Probability=1.000, F= 1.383 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06715, wR= 0.10557, Acormin=0.569, Acormax=1.427, Acor_av=0.960 F test: Probability=0.000, F= 0.960 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06842, wR= 0.10467, Acormin=0.529, Acormax=1.343, Acor_av=0.928 F test: Probability=0.000, F= 0.914 Final absorption model (ne=4, no=0): Rint= 0.06596, Acormin=0.587, Acormax=1.400, Acor_av=0.979 Combined refinement in use Rint: 0.18593 There are 41 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 0 (14 parameters) Refinement control: 54 pars with 1485 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.23464 Using Levenberg-Marquardt: 0.00010 New wR= 0.11769 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18383 with corrections 0.07172 Rint for all data: 0.18593 with corrections 0.07479 3 observations identified as outliers and rejected Cycle 2 wR= 0.08816 Using Levenberg-Marquardt: 0.00001 New wR= 0.07605 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17842 with corrections 0.05115 Rint for all data: 0.18593 with corrections 0.06124 1 observations identified as outliers and rejected Cycle 3 wR= 0.07038 Using Levenberg-Marquardt: 0.00000 New wR= 0.07047 Using Levenberg-Marquardt: 0.00001 New wR= 0.07047 Using Levenberg-Marquardt: 0.00010 New wR= 0.07047 Using Levenberg-Marquardt: 0.00100 New wR= 0.07047 Using Levenberg-Marquardt: 0.01000 New wR= 0.07045 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17775 with corrections 0.04996 Rint for all data: 0.18593 with corrections 0.06097 Final wR= 0.07045 Final frame scales: Min= 0.9078 Max= 1.2635 Final absorption correction factors: Amin= 0.6277 Amax= 1.3719 PROFFIT INFO: Inet (after scale3 abspack): min=-953.0378 max=1273319.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=61.2035 max=23440.6152 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/103 2814 reflections read from tmp file 112 reflections are rejected (111 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 6 9 4 4 5 3 3 122 Initial Chi^2= 0.52535 Cycle 1, Chi^2= 1.02350 Current error model SIG(F2)^2 = 67.80*I_RAW + 10.07*I_BACK+(0.03509*)^2 Cycle 2, Chi^2= 1.02730 Current error model SIG(F2)^2 = 87.38*I_RAW + 6.09*I_BACK+(0.02616*)^2 Cycle 3, Chi^2= 1.01822 Current error model SIG(F2)^2 = 98.05*I_RAW + 4.34*I_BACK+(0.02307*)^2 Cycle 4, Chi^2= 1.00833 Current error model SIG(F2)^2 = 102.90*I_RAW + 3.67*I_BACK+(0.02225*)^2 Cycle 5, Chi^2= 1.00308 Current error model SIG(F2)^2 = 104.77*I_RAW + 3.44*I_BACK+(0.02205*)^2 Cycle 6, Chi^2= 1.00106 Current error model SIG(F2)^2 = 105.43*I_RAW + 3.37*I_BACK+(0.02199*)^2 Cycle 7, Chi^2= 1.00036 Current error model SIG(F2)^2 = 105.65*I_RAW + 3.34*I_BACK+(0.02197*)^2 Cycle 8, Chi^2= 1.00012 Current error model SIG(F2)^2 = 105.73*I_RAW + 3.33*I_BACK+(0.02196*)^2 Final Chi^2= 1.00012 Final error model SIG(F2)^2 = 105.73*I_RAW + 3.33*I_BACK+(0.02196*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1273320- 125811 281 386778.37 33.32 100.00 125408- 3641 281 29457.03 12.32 100.00 3637- 2076 281 2816.55 5.61 98.22 2040- 1208 281 1570.04 3.69 55.52 1203- 822 281 984.66 2.51 16.01 822- 545 281 677.77 2.20 9.96 544- 329 281 430.29 1.87 7.83 327- 153 281 238.20 1.38 2.14 153- 17 281 80.20 0.76 0.36 17- -953 285 -145.04 -0.58 0.00 ------------------------------------------------------------------------------------ 1273320- -953 2814 42228.49 6.30 38.95 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 281 101599.20 10.32 70.82 1.64- 1.26 281 80627.66 9.81 60.50 1.26- 1.09 281 56500.50 8.28 68.68 1.09- 0.96 281 49847.81 6.73 33.10 0.96- 0.88 281 16800.94 4.73 46.26 0.88- 0.81 281 50065.39 7.68 38.08 0.81- 0.76 281 18651.65 3.87 19.57 0.76- 0.71 281 22510.34 5.01 18.51 0.71- 0.67 281 22367.10 4.94 27.76 0.67- 0.63 285 3860.45 1.69 6.67 ------------------------------------------------------------------------------------ 6.00- 0.63 2814 42228.49 6.30 38.95 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 281 101599.20 10.32 70.82 6.00- 1.26 562 91113.43 10.06 65.66 6.00- 1.09 843 79575.79 9.47 66.67 6.00- 0.96 1124 72143.79 8.78 58.27 6.00- 0.88 1405 61075.22 7.97 55.87 6.00- 0.81 1686 59240.25 7.92 52.91 6.00- 0.76 1967 53441.88 7.34 48.14 6.00- 0.71 2248 49575.44 7.05 44.44 6.00- 0.67 2529 46552.29 6.82 42.59 6.00- 0.63 2814 42228.49 6.30 38.95 ------------------------------------------------------------------------------------ 6.00- 0.63 2814 42228.49 6.30 38.95 Scale applied to data: s=0.785348 (maximum obs:1273319.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.061; Rsigma 0.036: data 2814 -> merged 162 With outlier rejection... Rint 0.048; Rsigma 0.036: data 2798 -> merged 162 Rejected total: 16, method kkm 13, method Blessing 3 Completeness direct cell (a, b, c) = (10.411, 10.411, 10.411), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626647, 6.010586 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.76 14 14 18.07 100.00 253 1.74 - 1.27 14 14 20.36 100.00 285 1.26 - 1.06 14 14 22.64 100.00 317 1.05 - 0.97 14 14 19.57 100.00 274 0.95 - 0.88 14 14 20.93 100.00 293 0.87 - 0.81 14 14 18.43 100.00 258 0.80 - 0.76 14 14 19.14 100.00 268 0.76 - 0.72 14 14 16.50 100.00 231 0.72 - 0.69 14 14 17.21 100.00 241 0.69 - 0.65 19 19 14.95 100.00 284 --------------------------------------------------------------- 7.37 - 0.65 145 145 18.65 100.00 2704 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:11:16 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.364025 7.363737 7.376201 120.2355 120.0592 89.7455 2737 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.39 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1390 1384 1384 1378 2079 1824 1824 2737 N (int>3sigma) = 0 154 157 217 153 264 403 411 599 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 21.7 24.0 23.4 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.1 4.6 4.4 Lattice type: P chosen Volume: 282.20 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.344 7.364 7.364 120.00 119.80 90.10 Niggli form: a.a = 53.930 b.b = 54.221 c.c = 54.225 b.c = -27.110 a.c = -26.873 a.b = -0.090 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.315 CUBIC F-lattice R(int) = 0.238 [ 2500] Vol = 1128.8 Cell: 10.437 10.408 10.391 89.85 90.00 89.90 Volume: 1128.80 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.458 TETRAGONAL I-lattice R(int) = 0.222 [ 2123] Vol = 564.4 Cell: 7.364 7.376 10.391 90.11 89.89 89.84 Volume: 564.40 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.350 TETRAGONAL I-lattice R(int) = 0.208 [ 2117] Vol = 564.4 Cell: 7.344 7.364 10.437 90.07 89.93 90.10 Volume: 564.40 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.124 TETRAGONAL I-lattice R(int) = 0.222 [ 2123] Vol = 564.4 Cell: 7.376 7.364 10.391 90.11 90.11 90.16 Volume: 564.40 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.415 ORTHORHOMBIC F-lattice R(int) = 0.181 [ 2084] Vol = 1128.8 Cell: 10.391 10.408 10.437 89.90 90.00 89.85 Volume: 1128.80 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.452 ORTHORHOMBIC I-lattice R(int) = 0.172 [ 2053] Vol = 564.4 Cell: 10.391 7.376 7.364 89.84 89.89 90.11 Volume: 564.40 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.129 ORTHORHOMBIC I-lattice R(int) = 0.211 [ 2056] Vol = 564.4 Cell: 7.344 7.364 10.437 89.93 90.07 90.10 Volume: 564.40 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.309 MONOCLINIC I-lattice R(int) = 0.112 [ 1586] Vol = 564.4 Cell: 7.364 10.391 7.376 90.11 90.16 90.11 Volume: 564.40 Matrix: 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.342 MONOCLINIC I-lattice R(int) = 0.177 [ 1580] Vol = 564.4 Cell: 7.364 10.408 7.364 89.96 90.25 89.82 Volume: 564.40 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.308 MONOCLINIC I-lattice R(int) = 0.112 [ 1586] Vol = 564.4 Cell: 7.376 10.391 7.364 90.11 90.16 90.11 Volume: 564.40 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.090 MONOCLINIC I-lattice R(int) = 0.189 [ 1544] Vol = 564.4 Cell: 7.344 7.364 10.437 90.07 90.07 89.90 Volume: 564.40 Matrix: 0.0000 1.0000 1.0000 1.0000 0.0000 1.0000 1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.065 MONOCLINIC I-lattice R(int) = 0.177 [ 1582] Vol = 564.4 Cell: 7.344 10.437 7.364 90.07 90.10 89.93 Volume: 564.40 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.093 MONOCLINIC I-lattice R(int) = 0.177 [ 1582] Vol = 564.4 Cell: 7.344 10.437 7.364 89.93 90.10 90.07 Volume: 564.40 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.111 [ 696] Vol = 282.2 Cell: 7.344 7.364 7.364 120.00 119.80 90.10 Volume: 282.20 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 1384 0 1817 1817 2737 N (int>3sigma) = 0 0 0 0 217 0 417 411 599 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 24.3 22.8 23.4 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.5 4.4 4.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.787 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 16 16 206 530 N I>3s 0 0 0 126 0.0 0.0 -0.0 1.6 0.5 0.5 0.1 2.5 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 0.238 2322 Fd-3m 1 1 227 C N N N N 37 2284 0.237 2385 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.437204 10.408261 10.390946 89.8457 90.0022 89.9034 ZERR 1.00 0.000982 0.010495 0.005676 0.0000 0.0001 0.1064 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1133257- 101792 338 328 27 12.1 340270.36 31.14 0.044 0.051 76822- 1752 539 535 27 19.8 5253.44 7.60 0.087 0.076 1664- 774 532 531 27 19.7 1192.59 2.86 0.234 0.288 769- 358 513 513 27 19.0 552.96 2.00 0.368 0.515 355- 74 486 486 27 18.0 237.98 1.15 0.566 0.939 63- -154 406 405 27 15.0 -5.37 0.12 0.960 3.599 ------------------------------------------------------------------------------------------- 1133257- -154 2814 2798 162 17.3 41261.50 6.23 0.048 0.054 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-1.27 540 536 27 19.9 91025.81 10.24 0.040 0.045 0.025 1.26-0.97 594 591 28 21.1 49846.53 7.12 0.042 0.052 0.032 0.95-0.81 553 551 28 19.7 33973.04 6.29 0.050 0.065 0.042 0.80-0.73 487 485 27 18.0 19199.64 4.23 0.058 0.067 0.055 0.72-0.67 425 424 27 15.7 19522.98 4.36 0.094 0.117 0.064 0.66-0.63 215 211 25 8.4 4226.73 1.77 0.089 0.050 0.126 ------------------------------------------------------------------------------------------------------ inf-0.63 2814 2798 162 17.3 41261.50 6.23 0.048 0.054 0.036 inf-0.65 2714 2702 144 18.8 42498.92 6.38 0.048 0.054 0.035 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-1.27 536 27 27 100.0 19.9 91025.81 43.68 0.040 0.009 1.26-0.97 591 28 28 100.0 21.1 49846.53 30.74 0.042 0.009 0.95-0.81 551 28 28 100.0 19.7 33973.04 27.61 0.050 0.011 0.80-0.73 485 27 27 100.0 18.0 19199.64 16.41 0.058 0.015 0.72-0.67 424 27 27 100.0 15.7 19522.98 18.37 0.094 0.017 0.66-0.63 211 25 25 100.0 8.4 4226.73 5.27 0.089 0.044 -------------------------------------------------------------------------------------------- inf-0.63 2798 162 162 100.0 17.3 41261.50 26.32 0.048 0.011 inf-0.65 2702 144 144 100.0 18.8 42498.92 27.11 0.048 0.010 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:17:51 2019) ID: 3668; threads 40; handles 811; mem 515472.00 (1204688.00)kB; time: 1w 4d 23h 28m 39s MEMORY INFO: Memory PF:275.0, Ph:652.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.4,peak PF: 700.2, WS: 471.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:276.0, Ph:654.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.2,peak PF: 700.2, WS: 473.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:17:51 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000097 0.000066 0.000097 ) 0.064809 0.092374 0.027273 ( 0.000109 0.000074 0.000108 ) 0.045523 0.057900 0.132205 ( 0.000131 0.000089 0.000130 ) 7.38096 ( 0.00718 ) 7.36649 ( 0.00753 ) 7.42630 ( 0.00861 ) 120.52449 ( 0.11594 ) 120.40327 ( 0.11299 ) 89.27095 ( 0.08083 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:17:51 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000097 0.000066 0.000097 ) 0.064809 0.092374 0.027273 ( 0.000109 0.000074 0.000108 ) 0.045523 0.057900 0.132205 ( 0.000131 0.000089 0.000130 ) M - matrix: 0.013818 0.004574 0.009180 ( 0.000025 0.000016 0.000022 ) 0.004574 0.014006 0.009362 ( 0.000016 0.000018 0.000018 ) 0.009180 0.009362 0.018511 ( 0.000022 0.000018 0.000035 ) unit cell: 7.381(7) 7.366(7) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | 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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb PROFFITPEAK info: 445 peaks in the peak location table UB fit with 57 obs out of 248 (total:248,skipped:0) (22.98%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 248 (total:248,skipped:0) (22.98%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087831 -0.044327 0.013040 ( 0.000064 0.000059 0.000074 ) 0.061747 0.094105 0.026060 ( 0.000046 0.000042 0.000053 ) 0.048770 0.055876 0.133072 ( 0.000066 0.000061 0.000077 ) M - matrix: 0.013905 0.004642 0.009244 ( 0.000014 0.000009 0.000012 ) 0.004642 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009244 0.009310 0.018557 ( 0.000012 0.000011 0.000021 ) UB fit with 232 obs out of 248 (total:248,skipped:0) (93.55%) unit cell: 7.355(5) 7.366(4) 7.361(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 232 obs out of 248 (total:248,skipped:0) (93.55%) UB - matrix: 0.087831 -0.044327 0.013040 ( 0.000064 0.000059 0.000074 ) 0.061747 0.094105 0.026060 ( 0.000046 0.000042 0.000053 ) 0.048770 0.055876 0.133072 ( 0.000066 0.000061 0.000077 ) M - matrix: 0.013905 0.004642 0.009244 ( 0.000014 0.000009 0.000012 ) 0.004642 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009244 0.009310 0.018557 ( 0.000012 0.000011 0.000021 ) unit cell: 7.355(5) 7.366(4) 7.361(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 248 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Run 3 Omega scan: (-48.000 - 52.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1264 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087831 -0.044327 0.013040 ( 0.000064 0.000059 0.000074 ) 0.061747 0.094105 0.026060 ( 0.000046 0.000042 0.000053 ) 0.048770 0.055876 0.133072 ( 0.000066 0.000061 0.000077 ) M - matrix: 0.013905 0.004642 0.009244 ( 0.000014 0.000009 0.000012 ) 0.004642 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009244 0.009310 0.018557 ( 0.000012 0.000011 0.000021 ) UB fit with 232 obs out of 248 (total:248,skipped:0) (93.55%) unit cell: 7.355(5) 7.366(4) 7.361(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 248 (total:248,skipped:0) (93.55%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb 0 of 233 peaks identified as outliers and rejected 233 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 233 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 233 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 23 | 0.865 ( 0.097) | 0.884 ( 0.140) | 1.257 ( 0.749) | 2.38- 1.76 | 23 | 0.895 ( 0.104) | 0.903 ( 0.156) | 1.035 ( 0.580) | 1.75- 1.58 | 23 | 0.911 ( 0.085) | 0.949 ( 0.117) | 0.774 ( 0.289) | 1.58- 1.36 | 23 | 0.944 ( 0.071) | 0.966 ( 0.130) | 0.884 ( 0.378) | 1.35- 1.19 | 23 | 0.956 ( 0.072) | 0.973 ( 0.132) | 0.934 ( 0.447) | 1.19- 1.06 | 23 | 0.977 ( 0.063) | 1.019 ( 0.112) | 0.958 ( 0.468) | 1.06- 0.89 | 23 | 1.000 ( 0.074) | 1.005 ( 0.124) | 1.060 ( 0.388) | 0.89- 0.82 | 23 | 0.981 ( 0.088) | 0.988 ( 0.104) | 0.925 ( 0.365) | 0.82- 0.72 | 23 | 1.001 ( 0.045) | 0.996 ( 0.127) | 1.231 ( 0.478) | 0.72- 0.63 | 26 | 0.976 ( 0.049) | 0.922 ( 0.124) | 1.218 ( 0.470) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 233 | 0.951 ( 0.088) | 0.960 ( 0.134) | 1.030 ( 0.502) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 233 obs out of 233 (total:233,skipped:0) (100.00%) UB - matrix: 0.087949 -0.044338 0.013018 ( 0.000033 0.000031 0.000038 ) 0.061813 0.094162 0.026120 ( 0.000021 0.000020 0.000024 ) 0.048818 0.055689 0.133252 ( 0.000036 0.000034 0.000041 ) M - matrix: 0.013939 0.004640 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004640 0.013934 0.009303 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009303 0.018608 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.344(2) 120.05(3) 119.84(3) 90.05(2) V = 281.16(16) OTKP changes: 233 1 1 1 OTKP changes: 233 1 1 1 OTKP changes: 233 1 1 1 UB - matrix: 0.087807 -0.044297 0.013073 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094153 0.026147 ( 0.000022 0.000021 0.000025 ) 0.048842 0.055806 0.133138 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013921 0.004660 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009313 0.018580 ( 0.000005 0.000005 0.000008 ) UB fit with 233 obs out of 233 (total:233,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3570(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 52.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1265 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087807 -0.044297 0.013073 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094153 0.026147 ( 0.000022 0.000021 0.000025 ) 0.048842 0.055806 0.133138 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013921 0.004660 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009313 0.018580 ( 0.000005 0.000005 0.000008 ) UB fit with 233 obs out of 233 (total:233,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3570(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 233 obs out of 233 (total:233,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.889 ( 0.110) | 0.898 ( 0.168) | 1.035 ( 0.560) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.133) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.957 ( 0.143) | 0.944 ( 0.509) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.88 | 24 | 0.968 ( 0.062) | 0.990 ( 0.103) | 1.122 ( 0.511) | 0.88- 0.79 | 24 | 1.011 ( 0.045) | 1.008 ( 0.130) | 0.982 ( 0.414) | 0.79- 0.69 | 24 | 0.996 ( 0.042) | 0.998 ( 0.130) | 1.258 ( 0.472) | 0.69- 0.63 | 20 | 0.975 ( 0.053) | 0.904 ( 0.105) | 1.267 ( 0.503) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 236 | 0.950 ( 0.085) | 0.960 ( 0.135) | 1.039 ( 0.520) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 70 | 0.979 ( 0.035) | 1.027 ( 0.076) | 1.150 ( 0.525) | 10.6-14.9 | 70 | 0.979 ( 0.044) | 1.039 ( 0.071) | 1.203 ( 0.551) | 14.9-18.8 | 70 | 0.997 ( 0.249) | 1.021 ( 0.103) | 1.282 ( 1.281) | 18.9-23.5 | 70 | 0.954 ( 0.055) | 1.002 ( 0.080) | 0.948 ( 0.435) | 23.5-26.8 | 70 | 0.962 ( 0.061) | 0.997 ( 0.100) | 0.978 ( 0.442) | 26.8-32.0 | 70 | 0.942 ( 0.090) | 0.949 ( 0.115) | 0.933 ( 0.475) | 32.1-36.3 | 70 | 0.928 ( 0.178) | 0.915 ( 0.136) | 1.055 ( 0.695) | 36.3-38.6 | 70 | 0.876 ( 0.096) | 0.841 ( 0.132) | 1.015 ( 0.504) | 38.6-41.7 | 70 | 0.889 ( 0.093) | 0.840 ( 0.126) | 1.069 ( 0.486) | 41.8-50.1 | 72 | 0.876 ( 0.111) | 0.800 ( 0.128) | 1.004 ( 0.509) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 702 | 0.938 ( 0.126) | 0.943 ( 0.138) | 1.063 ( 0.646) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.13 e2 dimension: a=-0.0071 b=1.25 e3 dimension: a=0.0006 b=1.07 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:18:02 2019 PROFFITMAIN - Started at Wed Aug 21 13:18:02 2019 OTKP changes: 306 2 2 3 OTKP changes: 306 2 2 3 OTKP changes: 306 2 2 3 UB - matrix: 0.087614 -0.046014 0.016828 ( 0.000089 0.000064 0.000090 ) 0.063486 0.092447 0.026890 ( 0.000105 0.000075 0.000106 ) 0.045346 0.057681 0.132076 ( 0.000107 0.000076 0.000108 ) M - matrix: 0.013763 0.004453 0.009171 ( 0.000023 0.000015 0.000018 ) 0.004453 0.013991 0.009330 ( 0.000015 0.000017 0.000016 ) 0.009171 0.009330 0.018450 ( 0.000018 0.000016 0.000029 ) UB fit with 353 obs out of 702 (total:702,skipped:0) (50.28%) unit cell: 7.395(7) 7.367(7) 7.430(7) 120.75(11) 120.31(10) 88.86(8) V = 284.4(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 201 obs out of 212 (total:212,skipped:0) (94.81%) UB - matrix: 0.087558 -0.046151 0.017208 ( 0.000107 0.000066 0.000101 ) 0.064647 0.092326 0.027114 ( 0.000088 0.000055 0.000083 ) 0.045862 0.057747 0.132082 ( 0.000105 0.000065 0.000099 ) M - matrix: 0.013949 0.004576 0.009317 ( 0.000024 0.000014 0.000018 ) 0.004576 0.013989 0.009337 ( 0.000014 0.000014 0.000014 ) 0.009317 0.009337 0.018477 ( 0.000018 0.000014 0.000027 ) unit cell: 7.375(7) 7.367(6) 7.437(7) 120.51(9) 120.48(10) 89.18(7) V = 283.5(4) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.145) HKL list info: 1285 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087481 -0.046151 0.017371 ( 0.000099 0.000062 0.000092 ) 0.064772 0.092369 0.027251 ( 0.000086 0.000053 0.000080 ) 0.045706 0.057843 0.132150 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013937 0.004589 0.009325 ( 0.000023 0.000013 0.000018 ) 0.004589 0.014008 0.009359 ( 0.000013 0.000014 0.000013 ) 0.009325 0.009359 0.018508 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.380(6) 7.366(6) 7.434(6) 120.52(9) 120.46(9) 89.22(7) V = 283.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 204 obs out of 212 (total:212,skipped:0) (96.23%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118023 0.039035 0.078676 ( 0.000076 0.000047 0.000070 ) 0.000074 0.111561 0.056284 ( 0.000079 0.000049 0.000073 ) -0.000028 -0.000071 0.095407 ( 0.000090 0.000056 0.000083 ) M - matrix: 0.013929 0.004615 0.009287 ( 0.000018 0.000011 0.000014 ) 0.004615 0.013970 0.009343 ( 0.000011 0.000012 0.000011 ) 0.009287 0.009343 0.018460 ( 0.000014 0.000011 0.000021 ) UB fit with 207 obs out of 212 (total:212,skipped:0) (97.64%) unit cell: 7.372(5) 7.379(5) 7.431(8) 120.48(9) 120.25(9) 89.47(6) V = 284.0(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087806 -0.044317 0.013059 ( 0.000032 0.000030 0.000036 ) 0.061850 0.094144 0.026133 ( 0.000022 0.000021 0.000025 ) 0.048846 0.055806 0.133152 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013921 0.004657 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004657 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009312 0.018583 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3558(19) 120.07(3) 119.86(3) 90.08(2) V = 281.86(14) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087795 -0.044316 0.013059 ( 0.000032 0.000030 0.000036 ) 0.061851 0.094143 0.026138 ( 0.000022 0.000021 0.000025 ) 0.048844 0.055812 0.133143 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004658 0.009266 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013942 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009266 0.009313 0.018581 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3568(19) 120.07(3) 119.86(3) 90.08(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 52.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1248 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087795 -0.044316 0.013059 ( 0.000032 0.000030 0.000036 ) 0.061851 0.094143 0.026138 ( 0.000022 0.000021 0.000025 ) 0.048844 0.055812 0.133143 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004658 0.009266 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013942 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009266 0.009313 0.018581 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3568(19) 120.07(3) 119.86(3) 90.08(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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: 0.087795 -0.044316 0.013059 ( 0.000032 0.000030 0.000036 ) 0.061851 0.094143 0.026138 ( 0.000022 0.000021 0.000025 ) 0.048844 0.055812 0.133143 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004658 0.009266 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013942 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009266 0.009313 0.018581 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3568(19) 120.07(3) 119.86(3) 90.08(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 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\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117827 0.038932 0.078593 ( 0.000038 0.000036 0.000044 ) 0.000059 0.111499 0.056155 ( 0.000028 0.000027 0.000033 ) -0.000091 -0.000146 0.096083 ( 0.000033 0.000032 0.000038 ) M - matrix: 0.013883 0.004594 0.009255 ( 0.000009 0.000005 0.000007 ) 0.004594 0.013948 0.009307 ( 0.000005 0.000007 0.000006 ) 0.009255 0.009307 0.018562 ( 0.000007 0.000006 0.000011 ) UB fit with 695 obs out of 702 (total:702,skipped:0) (99.00%) unit cell: 7.368(3) 7.363(2) 7.373(3) 120.21(4) 120.05(4) 89.71(3) V = 282.40(17) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 75 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof 3063 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:18:08 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.145) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 52.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-557.0000 max=7904045.0000 PROFFIT INFO: signal sum lp corr: min=-612.5250 max=1108672.4049 PROFFIT INFO: background sum: min=160.0000 max=7519.0000 PROFFIT INFO: background sum sig2: min=441.0000 max=5670.0000 PROFFIT INFO: num of signal pixels: min=44 max=501 PROFFIT INFO: Inet: min=-980.0400 max=1773875.8750 PROFFIT INFO: sig(Inet): min=58.9338 max=24369.0508 PROFFIT INFO: Inet/sig(Inet): min=-1.70 max=198.91 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 282 1061 1587 1910 2053 2382 2583 2701 2906 3030 3063 Percent 9.2 34.6 51.8 62.4 67.0 77.8 84.3 88.2 94.9 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3063 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 3063 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1773876- 129159 306 408661.18 76.75 100.00 129121- 4025 306 28809.66 19.71 100.00 4021- 2107 306 2911.32 7.21 98.69 2106- 1248 306 1614.57 3.84 53.27 1247- 821 306 1010.96 2.22 11.11 820- 538 306 680.23 1.67 7.19 537- 330 306 433.53 1.22 4.90 329- 154 306 239.03 0.73 1.63 153- 12 306 77.95 0.28 0.00 12- -980 309 -143.08 -0.28 0.00 ------------------------------------------------------------------------------------ 1773876- -980 3063 44385.88 11.32 37.64 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 306 101939.63 17.26 69.28 1.59- 1.22 306 86908.81 19.29 57.84 1.22- 1.02 306 59629.16 16.41 50.98 1.02- 0.89 306 35015.53 10.61 37.91 0.89- 0.81 306 29945.52 9.44 31.37 0.81- 0.73 306 46152.33 13.47 42.48 0.73- 0.66 306 26513.39 8.24 26.14 0.66- 0.61 306 20812.97 6.61 24.51 0.61- 0.56 306 22115.77 6.99 20.59 0.56- 0.44 309 15112.66 4.98 15.53 ------------------------------------------------------------------------------------ 6.55- 0.44 3063 44385.88 11.32 37.64 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:18:08 2019 Sorting 3063 observations 86 unique observations with > 7.00 F2/sig(F2) 3063 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 99 305 Total number of frames 305 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 3063 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 24 77 Total number of frames 77 736 observations > 7.00 F2/sig(F2) 736 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 24 77 Total number of frames 77 Removing 'redundancy=1' reflections Average redundancy: 5.9 (Out of 736 removed 36 = 700, unique = 119) 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 700 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 24 77 Total number of frames 77 119 unique data precomputed (should be 119) 119 unique data with 700 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.9 (Out of 700 removed 0 = 700, unique = 119) 119 unique data precomputed (should be 119) 119 unique data with 700 observations RMS deviation of equivalent data = 0.39164 Rint = 0.34597 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.34380, wR= 0.46780 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26352, wR= 0.35964, Acormin=0.522, Acormax=1.503, Acor_av=0.977 F test: Probability=1.000, F= 1.687 Trying model 2 (ne=2, no=1)... Results: Rint= 0.26646, wR= 0.36558, Acormin=0.237, Acormax=1.563, Acor_av=0.840 F test: Probability=0.000, F= 0.973 Trying model 3 (ne=4, no=0)... Results: Rint= 0.26206, wR= 0.35639, Acormin=0.523, Acormax=1.513, Acor_av=0.948 F test: Probability=0.000, F= 0.995 Trying model 4 (ne=4, no=1)... Results: Rint= 0.27171, wR= 0.37088, Acormin=0.170, Acormax=1.603, Acor_av=0.830 F test: Probability=0.000, F= 0.921 Trying model 5 (ne=4, no=3)... Results: Rint= 0.25701, wR= 0.35050, Acormin=0.203, Acormax=1.683, Acor_av=0.773 F test: Probability=0.577, F= 1.017 Trying model 6 (ne=6, no=0)... Results: Rint= 0.26225, wR= 0.33558, Acormin=0.211, Acormax=1.674, Acor_av=0.868 F test: Probability=0.000, F= 0.971 Trying model 7 (ne=6, no=1)... Results: Rint= 0.27285, wR= 0.34396, Acormin=-0.021, Acormax=1.702, Acor_av=0.804 F test: Probability=0.000, F= 0.892 Trying model 8 (ne=6, no=3)... Results: Rint= 0.26714, wR= 0.33306, Acormin=0.015, Acormax=1.606, Acor_av=0.725 F test: Probability=0.000, F= 0.919 Trying model 9 (ne=6, no=5)... Results: Rint= 0.34534, wR= 0.41889, Acormin=-0.078, Acormax=1.814, Acor_av=0.381 F test: Probability=0.000, F= 0.539 Trying model 10 (ne=8, no=0)... Results: Rint= 0.25496, wR= 0.31104, Acormin=0.097, Acormax=1.861, Acor_av=0.819 F test: Probability=0.000, F= 0.996 Trying model 11 (ne=8, no=1)... Results: Rint= 0.35092, wR= 0.42205, Acormin=-0.096, Acormax=1.269, Acor_av=0.436 F test: Probability=0.000, F= 0.523 Trying model 12 (ne=8, no=3)... Results: Rint= 0.31954, wR= 0.37769, Acormin=-0.007, Acormax=0.090, Acor_av=0.039 F test: Probability=0.000, F= 0.622 Trying model 13 (ne=8, no=5)... Results: Rint= 0.27634, wR= 0.33479, Acormin=-0.006, Acormax=0.100, Acor_av=0.043 F test: Probability=0.000, F= 0.814 Trying model 14 (ne=8, no=7)... Results: Rint= 0.18253, wR= 0.23960, Acormin=0.006, Acormax=0.119, Acor_av=0.048 F test: Probability=1.000, F= 1.812 Final absorption model (ne=2, no=0): Rint= 0.26352, Acormin=0.522, Acormax=1.503, Acor_av=0.977 Combined refinement in use Rint: 0.36043 There are 77 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 81 pars with 3321 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.39164 Using Levenberg-Marquardt: 0.00010 New wR= 0.22190 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34597 with corrections 0.19451 Rint for all data: 0.36043 with corrections 0.21069 0 observations identified as outliers and rejected Cycle 2 wR= 0.22190 Using Levenberg-Marquardt: 0.00001 New wR= 0.21519 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34597 with corrections 0.19113 Rint for all data: 0.36043 with corrections 0.20733 0 observations identified as outliers and rejected Cycle 3 wR= 0.21519 Using Levenberg-Marquardt: 0.00000 New wR= 0.21150 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34597 with corrections 0.19009 Rint for all data: 0.36043 with corrections 0.20628 0 observations identified as outliers and rejected Cycle 4 wR= 0.21150 Using Levenberg-Marquardt: 0.00000 New wR= 0.21327 Using Levenberg-Marquardt: 0.00000 New wR= 0.21327 Using Levenberg-Marquardt: 0.00001 New wR= 0.21327 Using Levenberg-Marquardt: 0.00010 New wR= 0.21326 Using Levenberg-Marquardt: 0.00100 New wR= 0.21312 Using Levenberg-Marquardt: 0.01000 New wR= 0.21233 Using Levenberg-Marquardt: 0.10000 New wR= 0.21134 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34597 with corrections 0.18947 Rint for all data: 0.36043 with corrections 0.20567 Final wR= 0.21134 Final frame scales: Min= 0.6048 Max= 2.1942 Final absorption correction factors: Amin= 0.4908 Amax= 1.4787 PROFFIT INFO: Inet (after scale3 abspack): min=-1625.7571 max=1677635.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=47.3078 max=30377.1074 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/103 3063 reflections read from tmp file 798 reflections are rejected (729 as outliers, 69 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 84 68 55 28 34 28 20 24 64 Initial Chi^2= 2.48184 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.82513 Current error model SIG(F2)^2 = 527.50*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 435.26*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 435.26*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1677635- 115276 306 376860.88 31.55 100.00 113976- 4045 306 25559.77 6.71 82.03 4037- 1998 306 2694.79 2.66 29.74 1996- 1136 306 1530.16 1.93 15.03 1135- 745 306 910.21 1.33 1.63 741- 484 306 605.35 1.10 0.00 483- 295 306 385.35 1.02 0.98 295- 142 306 216.49 0.82 0.65 141- 10 306 70.13 0.46 0.33 10- -1626 309 -167.19 -0.34 0.00 ------------------------------------------------------------------------------------ 1677635- -1626 3063 40826.40 4.72 23.02 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 306 105255.94 10.92 53.27 1.59- 1.22 306 80872.32 8.44 41.18 1.22- 1.02 306 58752.36 6.26 29.74 1.02- 0.89 306 31599.68 3.78 16.99 0.89- 0.81 306 26374.84 3.39 13.40 0.81- 0.73 306 41234.49 4.58 23.86 0.73- 0.66 306 21629.93 2.98 12.75 0.66- 0.61 306 16691.56 2.46 12.75 0.61- 0.56 306 16568.76 2.52 15.69 0.56- 0.44 309 9590.38 1.90 10.68 ------------------------------------------------------------------------------------ 6.55- 0.44 3063 40826.40 4.72 23.02 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 306 105255.94 10.92 53.27 6.55- 1.22 612 93064.13 9.68 47.22 6.55- 1.02 918 81626.87 8.54 41.39 6.55- 0.89 1224 69120.07 7.35 35.29 6.55- 0.81 1530 60571.03 6.56 30.92 6.55- 0.73 1836 57348.27 6.23 29.74 6.55- 0.66 2142 52245.65 5.76 27.31 6.55- 0.61 2448 47801.39 5.35 25.49 6.55- 0.56 2754 44331.10 5.04 24.40 6.55- 0.44 3063 40826.40 4.72 23.02 ------------------------------------------------------------------------------------ 6.55- 0.44 3063 40826.40 4.72 23.02 Scale applied to data: s=0.596077 (maximum obs:1677635.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.206; Rsigma 0.050: data 3063 -> merged 482 With outlier rejection... Rint 0.179; Rsigma 0.051: data 2974 -> merged 482 Rejected total: 89, method kkm 79, method Blessing 10 Completeness direct cell (a, b, c) = (6.561, 6.561, 6.561), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445374, 6.560776 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.59 22 22 15.00 100.00 330 1.55 - 1.22 22 22 13.55 100.00 298 1.20 - 1.02 22 22 12.27 100.00 270 1.02 - 0.92 22 22 10.45 100.00 230 0.92 - 0.84 22 22 10.18 100.00 224 0.84 - 0.79 22 22 8.27 100.00 182 0.79 - 0.75 22 22 8.45 100.00 186 0.75 - 0.71 22 22 6.82 100.00 150 0.71 - 0.69 22 22 7.09 100.00 156 0.68 - 0.65 26 29 6.73 89.66 175 --------------------------------------------------------------- 7.37 - 0.65 224 227 9.83 98.68 2201 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:18:08 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.367552 7.362617 7.373053 120.2112 120.0486 89.7125 2974 Reflections read from file xs2212a.hkl 2974 Reflections used for space-group determination (up to diffraction limit of 0.46A); mean (I/sigma) = 4.52 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1503 1503 1500 1491 2253 1982 1984 2974 N (int>3sigma) = 0 163 174 233 163 285 446 452 657 Mean intensity = 0.0 0.7 0.7 1.1 0.7 0.9 21.4 23.1 22.4 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.3 4.7 4.5 Lattice type: P chosen Volume: 282.40 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.344 7.363 7.365 119.92 90.12 119.82 Niggli form: a.a = 53.939 b.b = 54.208 c.c = 54.242 b.c = -27.043 a.c = -0.118 a.b = -26.893 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.277 CUBIC F-lattice R(int) = 0.223 [ 2738] Vol = 1129.6 Cell: 10.390 10.442 10.412 90.00 89.84 90.04 Volume: 1129.60 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.275 RHOMBOHEDRAL R-lattice R(int) = 0.211 [ 2310] Vol = 847.2 Cell: 7.363 7.344 18.060 89.91 90.17 119.82 Volume: 847.20 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.275 RHOMBOHEDRAL R-lattice R(int) = 0.190 [ 735] Vol = 847.2 Trigonal Cell: 7.363 7.344 18.060 89.91 90.17 119.82 Volume: 847.20 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.375 TETRAGONAL I-lattice R(int) = 0.215 [ 2356] Vol = 564.8 Cell: 7.373 7.373 10.390 89.86 89.91 90.16 Volume: 564.80 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.449 TETRAGONAL I-lattice R(int) = 0.215 [ 2356] Vol = 564.8 Cell: 7.373 7.373 10.390 89.86 89.91 90.16 Volume: 564.80 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.430 ORTHORHOMBIC I-lattice R(int) = 0.174 [ 2284] Vol = 564.8 Cell: 7.373 10.390 7.373 89.86 89.84 90.09 Volume: 564.80 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.282 MONOCLINIC I-lattice R(int) = 0.173 [ 1785] Vol = 564.8 Cell: 10.390 7.373 7.373 90.16 90.14 90.09 Volume: 564.80 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.141 MONOCLINIC I-lattice R(int) = 0.160 [ 1764] Vol = 564.8 Cell: 7.365 7.344 10.442 89.97 90.03 89.88 Volume: 564.80 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.077 MONOCLINIC C-lattice R(int) = 0.178 [ 1805] Vol = 564.8 Cell: 10.390 10.442 7.344 89.97 134.86 90.04 Volume: 564.80 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) = 0.113 [ 876] Vol = 282.4 Cell: 7.344 7.363 7.365 119.92 90.12 119.82 Volume: 282.40 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1500 0 1984 1973 2974 N (int>3sigma) = 0 0 0 0 233 0 452 459 657 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 23.1 23.3 22.4 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.7 4.6 4.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.779 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 224 566 N I>3s 0 0 0 135 0.0 0.0 -0.0 1.5 0.5 0.5 0.1 2.5 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 0.223 2542 Fd-3m 1 1 227 C N N N N 37 2284 0.224 2605 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.389638 10.441902 10.412316 90.0005 89.8397 90.0384 ZERR 1.00 0.006037 0.001018 0.011079 0.1083 0.0019 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 938884- 96440 333 303 48 6.3 347603.10 30.10 0.160 0.154 94171- 2601 400 382 48 8.0 11782.60 4.31 0.341 0.178 2559- 1499 490 479 48 10.0 1993.29 2.06 0.845 0.913 1470- 1017 481 473 48 9.9 1164.71 1.34 0.804 0.893 1014- 746 310 306 48 6.4 827.34 1.13 0.627 0.692 740- 559 295 287 48 6.0 606.94 0.93 0.686 0.747 556- 431 243 241 48 5.0 472.99 0.81 0.683 0.783 427- 302 184 178 48 3.7 339.83 0.72 0.659 0.782 294- 143 179 178 48 3.7 210.80 0.52 0.833 1.137 142- -288 148 147 50 2.9 45.02 0.15 0.945 2.468 ------------------------------------------------------------------------------------------- 938884- -288 3063 2974 482 6.2 37651.77 4.52 0.179 0.168 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-1.14 706 687 48 14.3 76725.40 8.59 0.178 0.170 0.028 1.14-0.89 565 551 51 10.8 40967.24 4.60 0.187 0.178 0.052 0.88-0.76 431 416 48 8.7 35195.76 4.09 0.191 0.188 0.068 0.76-0.69 367 359 49 7.3 26465.07 3.40 0.180 0.182 0.075 0.69-0.63 299 289 48 6.0 19800.20 2.74 0.176 0.172 0.095 0.63-0.59 241 231 49 4.7 10437.00 1.97 0.161 0.149 0.127 0.58-0.55 173 164 48 3.4 15066.07 2.33 0.132 0.129 0.111 0.55-0.52 127 124 51 2.4 5084.27 1.41 0.110 0.102 0.167 0.52-0.49 97 96 49 2.0 11473.85 2.23 0.063 0.064 0.115 0.49-0.45 57 57 41 1.4 3766.64 1.13 0.523 0.577 0.194 ------------------------------------------------------------------------------------------------------ inf-0.45 3063 2974 482 6.2 37651.77 4.52 0.179 0.168 0.051 inf-0.65 2264 2201 224 9.8 46132.23 5.33 0.181 0.174 0.045 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-1.14 687 48 48 100.0 14.3 76725.40 28.41 0.178 0.010 1.14-0.89 551 51 51 100.0 10.8 40967.24 13.55 0.187 0.023 0.88-0.76 416 48 48 100.0 8.7 35195.76 12.03 0.191 0.034 0.76-0.69 359 49 49 100.0 7.3 26465.07 9.15 0.180 0.033 0.69-0.63 289 51 48 94.1 6.0 19800.20 6.75 0.176 0.052 0.63-0.59 231 55 49 89.1 4.7 10437.00 4.12 0.161 0.065 0.58-0.55 164 55 48 87.3 3.4 15066.07 4.14 0.132 0.063 0.55-0.52 124 71 51 71.8 2.4 5084.27 2.12 0.110 0.097 0.52-0.49 96 81 49 60.5 2.0 11473.85 3.15 0.063 0.080 0.49-0.45 57 142 41 28.9 1.4 3766.64 1.33 0.523 0.923 -------------------------------------------------------------------------------------------- inf-0.45 2974 651 482 74.0 6.2 37651.77 13.28 0.179 0.030 inf-0.65 2201 227 224 98.7 9.8 46132.23 16.42 0.181 0.021 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.066418 0.012871 -0.008782 ( 0.000013 0.000014 0.000015 ) 0.014412 0.065208 -0.013260 ( 0.000012 0.000013 0.000014 ) 0.006077 -0.014655 -0.066253 ( 0.000016 0.000017 0.000018 ) M - matrix: 0.004656 -0.000004 -0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004632 -0.000007 ( 0.000001 0.000002 0.000002 ) -0.000010 -0.000007 0.004642 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.066418 0.012871 -0.008782 ( 0.000013 0.000014 0.000015 ) 0.014412 0.065208 -0.013260 ( 0.000012 0.000013 0.000014 ) 0.006077 -0.014655 -0.066253 ( 0.000016 0.000017 0.000018 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) unit cell: 10.395(2) 10.421(2) 10.410(2) 89.917(18) 89.871(17) 89.949(17) V = 1127.7(4) unit cell: 10.4088(6) 10.4088(6) 10.4088(6) 90.0 90.0 90.0 V = 1127.72(10) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.145) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 52.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-557.0000 max=7904045.0000 PROFFIT INFO: signal sum lp corr: min=-612.5250 max=1108672.4049 PROFFIT INFO: background sum: min=160.0000 max=7519.0000 PROFFIT INFO: background sum sig2: min=441.0000 max=5670.0000 PROFFIT INFO: num of signal pixels: min=44 max=501 PROFFIT INFO: Inet: min=-980.0400 max=1773875.8750 PROFFIT INFO: sig(Inet): min=58.9338 max=24369.0508 PROFFIT INFO: Inet/sig(Inet): min=-1.70 max=198.91 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 564 2122 3174 3820 4106 4764 5166 5402 5812 6060 6126 Percent 9.2 34.6 51.8 62.4 67.0 77.8 84.3 88.2 94.9 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3063 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 3063 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1773876- 129159 306 408661.18 76.75 100.00 129121- 4025 306 28809.66 19.71 100.00 4021- 2107 306 2911.32 7.21 98.69 2106- 1248 306 1614.57 3.84 53.27 1247- 821 306 1010.96 2.22 11.11 820- 538 306 680.23 1.67 7.19 537- 330 306 433.53 1.22 4.90 329- 154 306 239.03 0.73 1.63 153- 12 306 77.95 0.28 0.00 12- -980 309 -143.08 -0.28 0.00 ------------------------------------------------------------------------------------ 1773876- -980 3063 44385.88 11.32 37.64 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 306 110987.80 14.82 67.65 1.64- 1.26 306 83578.66 21.53 60.46 1.26- 1.09 306 59581.10 18.48 64.05 1.09- 0.96 306 52270.32 14.30 33.99 0.96- 0.88 306 15190.68 6.65 42.16 0.88- 0.81 306 54062.70 14.96 38.56 0.81- 0.76 306 19258.43 5.96 19.28 0.76- 0.71 306 22826.97 7.31 18.30 0.71- 0.67 306 22920.53 7.55 26.80 0.67- 0.63 309 3581.63 1.78 5.50 ------------------------------------------------------------------------------------ 6.00- 0.63 3063 44385.88 11.32 37.64 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:18:09 2019 Sorting 3063 observations 43 unique observations with > 7.00 F2/sig(F2) 3063 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 99 305 Total number of frames 305 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3063 observations in 3 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 Total number of frames 39 736 observations > 7.00 F2/sig(F2) 736 observations in 3 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 Total number of frames 39 Removing 'redundancy=1' reflections Average redundancy: 14.7 (Out of 736 removed 3 = 733, unique = 50) 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 733 observations in 3 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 Total number of frames 39 50 unique data precomputed (should be 50) 50 unique data with 733 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 14.7 (Out of 733 removed 0 = 733, unique = 50) 50 unique data precomputed (should be 50) 50 unique data with 733 observations RMS deviation of equivalent data = 0.26864 Rint = 0.18389 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17668, wR= 0.24082 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07864, wR= 0.13514, Acormin=0.602, Acormax=1.332, Acor_av=0.987 F test: Probability=1.000, F= 5.011 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07679, wR= 0.13127, Acormin=0.551, Acormax=1.359, Acor_av=0.958 F test: Probability=0.712, F= 1.044 Trying model 3 (ne=4, no=0)... Results: Rint= 0.07640, wR= 0.12597, Acormin=0.581, Acormax=1.388, Acor_av=0.959 F test: Probability=0.717, F= 1.045 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07617, wR= 0.12272, Acormin=0.541, Acormax=1.438, Acor_av=0.937 F test: Probability=0.723, F= 1.047 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07660, wR= 0.12138, Acormin=0.535, Acormax=1.375, Acor_av=0.910 F test: Probability=0.622, F= 1.024 Final absorption model (ne=2, no=0): Rint= 0.07864, Acormin=0.602, Acormax=1.332, Acor_av=0.987 Combined refinement in use Rint: 0.18602 There are 39 active scales (one needs to be fixed) Refinement control: frame scale #34 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 43 pars with 946 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26864 Using Levenberg-Marquardt: 0.00010 New wR= 0.14083 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18389 with corrections 0.08551 Rint for all data: 0.18602 with corrections 0.08841 4 observations identified as outliers and rejected Cycle 2 wR= 0.09650 Using Levenberg-Marquardt: 0.00001 New wR= 0.08677 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17489 with corrections 0.05897 Rint for all data: 0.18602 with corrections 0.07305 2 observations identified as outliers and rejected Cycle 3 wR= 0.07497 Using Levenberg-Marquardt: 0.00000 New wR= 0.07394 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17286 with corrections 0.05461 Rint for all data: 0.18602 with corrections 0.07189 1 observations identified as outliers and rejected Cycle 4 wR= 0.07122 Using Levenberg-Marquardt: 0.00000 New wR= 0.07003 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17213 with corrections 0.05268 Rint for all data: 0.18602 with corrections 0.07159 0 observations identified as outliers and rejected Cycle 5 wR= 0.07003 Using Levenberg-Marquardt: 0.00000 New wR= 0.06983 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17213 with corrections 0.05252 Rint for all data: 0.18602 with corrections 0.07144 0 observations identified as outliers and rejected Final wR= 0.06983 Final frame scales: Min= 0.9623 Max= 1.3106 Final absorption correction factors: Amin= 0.6690 Amax= 1.3994 PROFFIT INFO: Inet (after scale3 abspack): min=-965.1750 max=1237716.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=52.4133 max=25439.6074 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/103 3063 reflections read from tmp file 140 reflections are rejected (139 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 9 4 6 3 3 4 3 6 123 Initial Chi^2= 0.54544 Cycle 1, Chi^2= 1.03271 Current error model SIG(F2)^2 = 68.66*I_RAW + 9.88*I_BACK+(0.04332*)^2 Cycle 2, Chi^2= 1.02665 Current error model SIG(F2)^2 = 89.14*I_RAW + 6.04*I_BACK+(0.03426*)^2 Cycle 3, Chi^2= 1.02171 Current error model SIG(F2)^2 = 102.25*I_RAW + 3.95*I_BACK+(0.02945*)^2 Cycle 4, Chi^2= 1.01620 Current error model SIG(F2)^2 = 110.71*I_RAW + 2.79*I_BACK+(0.02688*)^2 Cycle 5, Chi^2= 1.01046 Current error model SIG(F2)^2 = 115.88*I_RAW + 2.17*I_BACK+(0.02557*)^2 Cycle 6, Chi^2= 1.00584 Current error model SIG(F2)^2 = 118.80*I_RAW + 1.87*I_BACK+(0.02493*)^2 Cycle 7, Chi^2= 1.00294 Current error model SIG(F2)^2 = 120.32*I_RAW + 1.73*I_BACK+(0.02463*)^2 Cycle 8, Chi^2= 1.00140 Current error model SIG(F2)^2 = 121.05*I_RAW + 1.67*I_BACK+(0.02449*)^2 Cycle 9, Chi^2= 1.00065 Current error model SIG(F2)^2 = 121.40*I_RAW + 1.64*I_BACK+(0.02443*)^2 Cycle 10, Chi^2= 1.00030 Current error model SIG(F2)^2 = 121.56*I_RAW + 1.62*I_BACK+(0.02440*)^2 Final Chi^2= 1.00030 Final error model SIG(F2)^2 = 121.56*I_RAW + 1.62*I_BACK+(0.02440*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1237716- 124472 306 389865.33 30.83 100.00 124456- 3736 306 29658.15 11.43 100.00 3722- 2067 306 2818.17 5.23 96.73 2058- 1211 306 1562.36 3.42 46.41 1209- 818 306 981.40 2.37 13.07 817- 542 306 672.40 2.06 8.17 542- 333 306 428.82 1.81 8.17 332- 155 306 236.95 1.39 1.31 152- 12 306 76.93 0.74 0.33 12- -965 309 -146.65 -0.59 0.00 ------------------------------------------------------------------------------------ 1237716- -965 3063 42573.50 5.86 37.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 306 105664.52 9.65 68.63 1.64- 1.26 306 78824.23 9.05 60.13 1.26- 1.09 306 59218.50 7.74 65.36 1.09- 0.96 306 49566.36 6.30 33.33 0.96- 0.88 306 14571.94 4.17 41.83 0.88- 0.81 306 52108.93 7.43 37.91 0.81- 0.76 306 18722.40 3.60 17.32 0.76- 0.71 306 21544.09 4.58 17.97 0.71- 0.67 306 22313.71 4.62 26.14 0.67- 0.63 309 3582.61 1.52 5.50 ------------------------------------------------------------------------------------ 6.00- 0.63 3063 42573.50 5.86 37.38 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 306 105664.52 9.65 68.63 6.00- 1.26 612 92244.38 9.35 64.38 6.00- 1.09 918 81235.75 8.82 64.71 6.00- 0.96 1224 73318.40 8.19 56.86 6.00- 0.88 1530 61569.11 7.38 53.86 6.00- 0.81 1836 59992.41 7.39 51.20 6.00- 0.76 2142 54096.70 6.85 46.36 6.00- 0.71 2448 50027.62 6.57 42.81 6.00- 0.67 2754 46948.30 6.35 40.96 6.00- 0.63 3063 42573.50 5.86 37.38 ------------------------------------------------------------------------------------ 6.00- 0.63 3063 42573.50 5.86 37.38 Scale applied to data: s=0.807939 (maximum obs:1237716.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.071; Rsigma 0.038: data 3063 -> merged 162 With outlier rejection... Rint 0.054; Rsigma 0.038: data 3049 -> merged 162 Rejected total: 14, method kkm 10, method Blessing 4 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626536, 6.009527 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.76 14 14 19.79 100.00 277 1.73 - 1.27 14 14 22.36 100.00 313 1.26 - 1.06 14 14 24.64 100.00 345 1.05 - 0.97 14 14 21.36 100.00 299 0.95 - 0.88 14 14 22.79 100.00 319 0.87 - 0.81 14 14 19.86 100.00 278 0.80 - 0.76 14 14 21.00 100.00 294 0.76 - 0.72 14 14 17.86 100.00 250 0.72 - 0.69 14 14 18.79 100.00 263 0.69 - 0.65 19 19 16.37 100.00 311 --------------------------------------------------------------- 7.37 - 0.65 145 145 20.34 100.00 2949 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:18:08 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.367552 7.362617 7.373053 120.2112 120.0486 89.7125 2974 Reflections read from file xs2212a.hkl 2974 Reflections used for space-group determination (up to diffraction limit of 0.46A); mean (I/sigma) = 4.52 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1503 1503 1500 1491 2253 1982 1984 2974 N (int>3sigma) = 0 163 174 233 163 285 446 452 657 Mean intensity = 0.0 0.7 0.7 1.1 0.7 0.9 21.4 23.1 22.4 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.3 4.7 4.5 Lattice type: P chosen Volume: 282.40 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.344 7.363 7.365 119.92 90.12 119.82 Niggli form: a.a = 53.939 b.b = 54.208 c.c = 54.242 b.c = -27.043 a.c = -0.118 a.b = -26.893 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.277 CUBIC F-lattice R(int) = 0.223 [ 2738] Vol = 1129.6 Cell: 10.390 10.442 10.412 90.00 89.84 90.04 Volume: 1129.60 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.275 RHOMBOHEDRAL R-lattice R(int) = 0.211 [ 2310] Vol = 847.2 Cell: 7.363 7.344 18.060 89.91 90.17 119.82 Volume: 847.20 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.275 RHOMBOHEDRAL R-lattice R(int) = 0.190 [ 735] Vol = 847.2 Trigonal Cell: 7.363 7.344 18.060 89.91 90.17 119.82 Volume: 847.20 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.375 TETRAGONAL I-lattice R(int) = 0.215 [ 2356] Vol = 564.8 Cell: 7.373 7.373 10.390 89.86 89.91 90.16 Volume: 564.80 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.449 TETRAGONAL I-lattice R(int) = 0.215 [ 2356] Vol = 564.8 Cell: 7.373 7.373 10.390 89.86 89.91 90.16 Volume: 564.80 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.430 ORTHORHOMBIC I-lattice R(int) = 0.174 [ 2284] Vol = 564.8 Cell: 7.373 10.390 7.373 89.86 89.84 90.09 Volume: 564.80 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.282 MONOCLINIC I-lattice R(int) = 0.173 [ 1785] Vol = 564.8 Cell: 10.390 7.373 7.373 90.16 90.14 90.09 Volume: 564.80 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.141 MONOCLINIC I-lattice R(int) = 0.160 [ 1764] Vol = 564.8 Cell: 7.365 7.344 10.442 89.97 90.03 89.88 Volume: 564.80 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.077 MONOCLINIC C-lattice R(int) = 0.178 [ 1805] Vol = 564.8 Cell: 10.390 10.442 7.344 89.97 134.86 90.04 Volume: 564.80 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) = 0.113 [ 876] Vol = 282.4 Cell: 7.344 7.363 7.365 119.92 90.12 119.82 Volume: 282.40 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1500 0 1984 1973 2974 N (int>3sigma) = 0 0 0 0 233 0 452 459 657 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 23.1 23.3 22.4 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.7 4.6 4.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.779 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 224 566 N I>3s 0 0 0 135 0.0 0.0 -0.0 1.5 0.5 0.5 0.1 2.5 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 0.223 2542 Fd-3m 1 1 227 C N N N N 37 2284 0.224 2605 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.389638 10.441902 10.412316 90.0005 89.8397 90.0384 ZERR 1.00 0.006037 0.001018 0.011079 0.1083 0.0019 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1134885- 102876 370 361 27 13.4 341716.19 28.76 0.050 0.060 75456- 1725 576 573 27 21.2 5486.36 7.26 0.106 0.137 1720- 791 599 598 27 22.1 1189.76 2.61 0.231 0.291 771- 359 556 556 27 20.6 540.97 1.82 0.379 0.527 356- 62 545 545 27 20.2 225.85 1.13 0.555 0.869 59- -181 417 416 27 15.4 -4.96 0.10 0.966 3.779 ------------------------------------------------------------------------------------------- 1134885- -181 3063 3049 162 18.8 41861.76 5.83 0.054 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-1.27 593 588 27 21.8 92240.41 9.51 0.043 0.050 0.028 1.26-0.97 615 612 27 22.7 53822.40 6.94 0.048 0.063 0.034 0.97-0.81 617 615 28 22.0 33098.51 5.76 0.057 0.071 0.045 0.81-0.73 531 530 27 19.6 15660.75 3.48 0.078 0.094 0.062 0.73-0.67 475 474 28 16.9 22720.78 4.54 0.091 0.112 0.065 0.66-0.63 232 230 25 9.2 4497.46 1.71 0.158 0.102 0.130 ------------------------------------------------------------------------------------------------------ inf-0.63 3063 3049 162 18.8 41861.76 5.83 0.054 0.064 0.038 inf-0.65 2959 2947 144 20.5 43058.31 5.96 0.053 0.062 0.038 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-1.27 588 27 27 100.0 21.8 92240.41 42.33 0.043 0.009 1.26-0.97 612 27 27 100.0 22.7 53822.40 31.39 0.048 0.009 0.97-0.81 615 28 28 100.0 22.0 33098.51 27.10 0.057 0.012 0.81-0.73 530 27 27 100.0 19.6 15660.75 14.37 0.078 0.017 0.73-0.67 474 28 28 100.0 16.9 22720.78 19.60 0.091 0.017 0.66-0.63 230 25 25 100.0 9.2 4497.46 5.42 0.158 0.047 -------------------------------------------------------------------------------------------- inf-0.63 3049 162 162 100.0 18.8 41861.76 25.88 0.054 0.012 inf-0.65 2947 144 144 100.0 20.5 43058.31 26.62 0.053 0.011 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:19:11 2019) ID: 3668; threads 40; handles 810; mem 514904.00 (1204688.00)kB; time: 1w 4d 23h 29m 59s MEMORY INFO: Memory PF:273.0, Ph:646.0, V:1176.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:502.8,peak PF: 700.2, WS: 470.8, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:274.0, Ph:647.0, V:1179.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:504.6,peak PF: 700.2, WS: 472.6, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:19:11 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000095 0.000066 0.000095 ) 0.064809 0.092374 0.027273 ( 0.000111 0.000077 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000134 0.000093 0.000134 ) 7.38096 ( 0.00717 ) 7.36649 ( 0.00765 ) 7.42630 ( 0.00885 ) 120.52449 ( 0.11863 ) 120.40327 ( 0.11480 ) 89.27095 ( 0.08139 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:19:11 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000095 0.000066 0.000095 ) 0.064809 0.092374 0.027273 ( 0.000111 0.000077 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000134 0.000093 0.000134 ) M - matrix: 0.013792 0.004558 0.009163 ( 0.000025 0.000016 0.000022 ) 0.004558 0.013996 0.009353 ( 0.000016 0.000019 0.000018 ) 0.009163 0.009353 0.018507 ( 0.000022 0.000018 0.000036 ) unit cell: 7.381(7) 7.366(8) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 211 peaks identified as outliers and rejected 211 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 211 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 211 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 22 | 0.950 ( 0.039) | 0.934 ( 0.098) | 1.377 ( 0.482) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 211 | 0.942 ( 0.193) | 0.948 ( 0.158) | 1.105 ( 0.893) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.908 ( 0.086) | 0.911 ( 0.142) | 0.971 ( 0.421) | 1.58- 1.35 | 25 | 0.950 ( 0.070) | 0.967 ( 0.106) | 0.862 ( 0.454) | 1.35- 1.19 | 25 | 0.920 ( 0.067) | 0.919 ( 0.118) | 1.018 ( 0.602) | 1.19- 1.09 | 25 | 0.928 ( 0.064) | 0.973 ( 0.087) | 0.831 ( 0.287) | 1.06- 0.92 | 25 | 0.964 ( 0.065) | 0.985 ( 0.097) | 1.124 ( 0.459) | 0.91- 0.86 | 25 | 0.942 ( 0.069) | 0.940 ( 0.092) | 1.023 ( 0.391) | 0.82- 0.73 | 25 | 0.957 ( 0.051) | 0.912 ( 0.087) | 1.320 ( 0.421) | 0.73- 0.63 | 28 | 0.930 ( 0.038) | 0.881 ( 0.096) | 1.353 ( 0.465) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 253 | 0.925 ( 0.077) | 0.924 ( 0.117) | 1.054 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb PROFFITPEAK info: 452 peaks in the peak location table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.82 | 24 | 1.005 ( 0.047) | 1.008 ( 0.130) | 0.907 ( 0.354) | 0.79- 0.69 | 24 | 0.998 ( 0.044) | 1.006 ( 0.137) | 1.289 ( 0.497) | 0.69- 0.63 | 23 | 0.979 ( 0.051) | 0.913 ( 0.103) | 1.157 ( 0.432) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.510) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 70 | 0.979 ( 0.036) | 1.026 ( 0.076) | 1.150 ( 0.524) | 10.6-14.9 | 70 | 0.979 ( 0.044) | 1.039 ( 0.071) | 1.203 ( 0.551) | 14.9-18.8 | 70 | 0.997 ( 0.249) | 1.021 ( 0.103) | 1.282 ( 1.281) | 18.9-23.4 | 70 | 0.955 ( 0.055) | 1.004 ( 0.079) | 0.936 ( 0.433) | 23.5-26.7 | 70 | 0.960 ( 0.061) | 0.997 ( 0.100) | 0.977 ( 0.442) | 26.8-31.9 | 70 | 0.942 ( 0.090) | 0.947 ( 0.113) | 0.932 ( 0.475) | 32.0-36.2 | 70 | 0.933 ( 0.177) | 0.921 ( 0.136) | 1.038 ( 0.693) | 36.2-38.6 | 70 | 0.873 ( 0.095) | 0.840 ( 0.129) | 1.025 ( 0.507) | 38.6-41.6 | 70 | 0.894 ( 0.095) | 0.846 ( 0.134) | 1.049 ( 0.455) | 41.7-50.1 | 73 | 0.877 ( 0.110) | 0.802 ( 0.125) | 1.005 ( 0.509) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 703 | 0.939 ( 0.126) | 0.944 ( 0.138) | 1.059 ( 0.644) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.13 e2 dimension: a=-0.0071 b=1.25 e3 dimension: a=0.0002 b=1.08 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3517 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:19:22 2019 PROFFITMAIN - Started at Wed Aug 21 13:19:22 2019 OTKP changes: 305 2 2 3 OTKP changes: 305 2 2 3 OTKP changes: 305 2 2 3 UB - matrix: 0.087616 -0.046033 0.016817 ( 0.000090 0.000064 0.000091 ) 0.063485 0.092450 0.026881 ( 0.000104 0.000074 0.000104 ) 0.045393 0.057643 0.132050 ( 0.000105 0.000076 0.000106 ) M - matrix: 0.013767 0.004453 0.009174 ( 0.000023 0.000015 0.000018 ) 0.004453 0.013989 0.009323 ( 0.000015 0.000017 0.000016 ) 0.009174 0.009323 0.018443 ( 0.000018 0.000016 0.000029 ) UB fit with 353 obs out of 703 (total:703,skipped:0) (50.21%) unit cell: 7.395(7) 7.366(7) 7.431(7) 120.73(10) 120.33(10) 88.85(8) V = 284.4(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 202 obs out of 211 (total:211,skipped:0) (95.73%) UB - matrix: 0.087570 -0.046158 0.017186 ( 0.000108 0.000067 0.000100 ) 0.064672 0.092317 0.027118 ( 0.000087 0.000054 0.000080 ) 0.045907 0.057730 0.132124 ( 0.000107 0.000066 0.000098 ) M - matrix: 0.013958 0.004578 0.009324 ( 0.000024 0.000014 0.000018 ) 0.004578 0.013986 0.009338 ( 0.000014 0.000014 0.000014 ) 0.009324 0.009338 0.018487 ( 0.000018 0.000014 0.000027 ) unit cell: 7.373(7) 7.368(6) 7.435(7) 120.50(9) 120.48(10) 89.19(7) V = 283.4(4) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.143) HKL list info: 1284 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087518 -0.046167 0.017343 ( 0.000101 0.000063 0.000093 ) 0.064780 0.092376 0.027248 ( 0.000084 0.000052 0.000078 ) 0.045782 0.057833 0.132131 ( 0.000105 0.000065 0.000097 ) M - matrix: 0.013952 0.004591 0.009332 ( 0.000023 0.000013 0.000018 ) 0.004591 0.014009 0.009358 ( 0.000013 0.000014 0.000013 ) 0.009332 0.009358 0.018502 ( 0.000018 0.000013 0.000026 ) UB fit with 199 obs out of 211 (total:211,skipped:0) (94.31%) unit cell: 7.378(6) 7.365(6) 7.437(6) 120.52(9) 120.49(9) 89.20(7) V = 283.3(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 204 obs out of 211 (total:211,skipped:0) (96.68%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118012 0.039044 0.078730 ( 0.000074 0.000046 0.000068 ) 0.000070 0.111566 0.056248 ( 0.000078 0.000049 0.000072 ) -0.000089 -0.000064 0.095406 ( 0.000089 0.000055 0.000082 ) M - matrix: 0.013927 0.004615 0.009287 ( 0.000018 0.000011 0.000014 ) 0.004615 0.013971 0.009343 ( 0.000011 0.000011 0.000011 ) 0.009287 0.009343 0.018464 ( 0.000014 0.000011 0.000021 ) UB fit with 206 obs out of 211 (total:211,skipped:0) (97.63%) unit cell: 7.373(5) 7.378(5) 7.429(8) 120.47(9) 120.24(9) 89.48(6) V = 283.9(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045186 0.014002 ( 0.000045 0.000055 0.000057 ) 0.062040 0.093035 0.025392 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133668 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009279 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.05(5) 89.65(4) V = 281.7(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087463 -0.045178 0.013978 ( 0.000045 0.000055 0.000058 ) 0.062035 0.093004 0.025377 ( 0.000037 0.000045 0.000047 ) 0.048449 0.057033 0.133640 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013845 0.004581 0.009271 ( 0.000010 0.000007 0.000007 ) 0.004581 0.013944 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009271 0.009351 0.018699 ( 0.000007 0.000007 0.000010 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.349(3) 120.28(5) 120.04(5) 89.66(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1304 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087463 -0.045178 0.013978 ( 0.000045 0.000055 0.000058 ) 0.062035 0.093004 0.025377 ( 0.000037 0.000045 0.000047 ) 0.048449 0.057033 0.133640 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013845 0.004581 0.009271 ( 0.000010 0.000007 0.000007 ) 0.004581 0.013944 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009271 0.009351 0.018699 ( 0.000007 0.000007 0.000010 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.349(3) 120.28(5) 120.04(5) 89.66(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117816 0.039148 0.078861 ( 0.000032 0.000039 0.000041 ) 0.000016 0.111463 0.056243 ( 0.000035 0.000042 0.000044 ) -0.000040 -0.000029 0.096440 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013881 0.004614 0.009288 ( 0.000008 0.000006 0.000006 ) 0.004614 0.013957 0.009353 ( 0.000006 0.000010 0.000007 ) 0.009288 0.009353 0.018683 ( 0.000006 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.370(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.68(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.087804 -0.044309 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094149 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055798 0.133161 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004658 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009312 0.018585 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3551(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1267 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117826 0.038927 0.078622 ( 0.000038 0.000037 0.000044 ) 0.000066 0.111491 0.056135 ( 0.000027 0.000026 0.000032 ) -0.000102 -0.000138 0.096092 ( 0.000033 0.000031 0.000038 ) M - matrix: 0.013883 0.004594 0.009258 ( 0.000009 0.000005 0.000007 ) 0.004594 0.013946 0.009306 ( 0.000005 0.000006 0.000006 ) 0.009258 0.009306 0.018566 ( 0.000007 0.000006 0.000011 ) UB fit with 696 obs out of 703 (total:703,skipped:0) (99.00%) unit cell: 7.368(3) 7.363(2) 7.372(3) 120.20(4) 120.06(4) 89.72(3) V = 282.40(17) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 73 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof 3083 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:19:27 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.143) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-560.0000 max=7943967.0000 PROFFIT INFO: signal sum lp corr: min=-576.8383 max=1106771.8949 PROFFIT INFO: background sum: min=160.0000 max=7577.0000 PROFFIT INFO: background sum sig2: min=441.0000 max=5482.0000 PROFFIT INFO: num of signal pixels: min=43 max=485 PROFFIT INFO: Inet: min=-922.9413 max=1770835.0000 PROFFIT INFO: sig(Inet): min=57.2785 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.68 max=197.75 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 273 1059 1582 1918 2064 2394 2598 2716 2919 3049 3083 Percent 8.9 34.3 51.3 62.2 66.9 77.7 84.3 88.1 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3083 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 3083 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1770835- 132485 308 411481.60 77.66 100.00 132366- 4113 308 30831.21 19.97 100.00 4103- 2134 308 2936.11 7.30 98.70 2129- 1256 308 1633.60 3.87 52.92 1255- 834 308 1021.70 2.24 12.01 834- 555 308 688.58 1.68 7.14 555- 331 308 438.34 1.27 5.84 331- 156 308 242.33 0.73 1.62 156- 19 308 83.96 0.29 0.00 18- -923 311 -142.02 -0.27 0.00 ------------------------------------------------------------------------------------ 1770835- -923 3083 44877.69 11.46 37.79 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 308 101596.61 17.23 68.83 1.59- 1.22 308 87362.49 19.59 59.09 1.22- 1.02 308 60522.27 16.57 50.65 1.02- 0.89 308 36051.73 10.82 38.31 0.89- 0.81 308 29893.06 9.43 31.49 0.80- 0.73 308 47884.25 13.89 42.86 0.73- 0.66 308 26484.65 8.22 25.32 0.66- 0.61 308 20833.28 6.60 24.35 0.61- 0.56 308 22315.03 7.04 20.78 0.56- 0.44 311 16113.70 5.30 16.40 ------------------------------------------------------------------------------------ 6.55- 0.44 3083 44877.69 11.46 37.79 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:19:27 2019 Sorting 3083 observations 87 unique observations with > 7.00 F2/sig(F2) 3083 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 Total number of frames 307 Maximum number of 87 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 3083 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 25 78 Total number of frames 78 745 observations > 7.00 F2/sig(F2) 745 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 25 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 5.9 (Out of 745 removed 35 = 710, unique = 120) 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 710 observations in 3 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 25 78 Total number of frames 78 120 unique data precomputed (should be 120) 120 unique data with 710 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.9 (Out of 710 removed 0 = 710, unique = 120) 120 unique data precomputed (should be 120) 120 unique data with 710 observations RMS deviation of equivalent data = 0.37460 Rint = 0.33466 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.33261, wR= 0.44388 Trying model 1 (ne=2, no=0)... Results: Rint= 0.25484, wR= 0.33793, Acormin=0.541, Acormax=1.472, Acor_av=0.981 F test: Probability=1.000, F= 1.689 Trying model 2 (ne=2, no=1)... Results: Rint= 0.25524, wR= 0.34437, Acormin=0.334, Acormax=1.494, Acor_av=0.862 F test: Probability=0.000, F= 0.992 Trying model 3 (ne=4, no=0)... Results: Rint= 0.25121, wR= 0.33230, Acormin=0.539, Acormax=1.439, Acor_av=0.963 F test: Probability=0.563, F= 1.013 Trying model 4 (ne=4, no=1)... Results: Rint= 0.25517, wR= 0.34327, Acormin=0.276, Acormax=1.538, Acor_av=0.861 F test: Probability=0.000, F= 0.977 Trying model 5 (ne=4, no=3)... Results: Rint= 0.23816, wR= 0.31771, Acormin=0.252, Acormax=1.562, Acor_av=0.814 F test: Probability=0.890, F= 1.108 Trying model 6 (ne=6, no=0)... Results: Rint= 0.24979, wR= 0.31169, Acormin=0.243, Acormax=1.650, Acor_av=0.888 F test: Probability=0.508, F= 1.002 Trying model 7 (ne=6, no=1)... Results: Rint= 0.25582, wR= 0.31746, Acormin=0.069, Acormax=1.621, Acor_av=0.836 F test: Probability=0.000, F= 0.950 Trying model 8 (ne=6, no=3)... Results: Rint= 0.24697, wR= 0.30109, Acormin=0.066, Acormax=1.558, Acor_av=0.771 F test: Probability=0.530, F= 1.006 Trying model 9 (ne=6, no=5)... Results: Rint= 0.30425, wR= 0.36861, Acormin=-0.030, Acormax=1.694, Acor_av=0.425 F test: Probability=0.000, F= 0.650 Trying model 10 (ne=8, no=0)... Results: Rint= 0.24016, wR= 0.28946, Acormin=0.154, Acormax=1.875, Acor_av=0.847 F test: Probability=0.721, F= 1.051 Trying model 11 (ne=8, no=1)... Results: Rint= 0.32442, wR= 0.39499, Acormin=-0.046, Acormax=1.325, Acor_av=0.473 F test: Probability=0.000, F= 0.573 Trying model 12 (ne=8, no=3)... Results: Rint= 0.27200, wR= 0.32604, Acormin=-0.003, Acormax=0.102, Acor_av=0.048 F test: Probability=0.000, F= 0.804 Trying model 13 (ne=8, no=5)... Results: Rint= 0.23671, wR= 0.29029, Acormin=0.002, Acormax=0.117, Acor_av=0.055 F test: Probability=0.677, F= 1.040 Trying model 14 (ne=8, no=7)... Results: Rint= 0.16064, wR= 0.20957, Acormin=0.014, Acormax=0.158, Acor_av=0.063 F test: Probability=1.000, F= 2.193 Final absorption model (ne=2, no=0): Rint= 0.25484, Acormin=0.541, Acormax=1.472, Acor_av=0.981 Combined refinement in use Rint: 0.34902 There are 78 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 82 pars with 3403 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.37460 Using Levenberg-Marquardt: 0.00010 New wR= 0.21363 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33466 with corrections 0.19102 Rint for all data: 0.34902 with corrections 0.20699 0 observations identified as outliers and rejected Cycle 2 wR= 0.21363 Using Levenberg-Marquardt: 0.00001 New wR= 0.20617 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33466 with corrections 0.18156 Rint for all data: 0.34902 with corrections 0.19765 0 observations identified as outliers and rejected Cycle 3 wR= 0.20617 Using Levenberg-Marquardt: 0.00000 New wR= 0.20277 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33466 with corrections 0.18103 Rint for all data: 0.34902 with corrections 0.19704 0 observations identified as outliers and rejected Cycle 4 wR= 0.20277 Using Levenberg-Marquardt: 0.00000 New wR= 0.20317 Using Levenberg-Marquardt: 0.00000 New wR= 0.20317 Using Levenberg-Marquardt: 0.00001 New wR= 0.20317 Using Levenberg-Marquardt: 0.00010 New wR= 0.20317 Using Levenberg-Marquardt: 0.00100 New wR= 0.20315 Using Levenberg-Marquardt: 0.01000 New wR= 0.20305 Using Levenberg-Marquardt: 0.10000 New wR= 0.20292 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33466 with corrections 0.18113 Rint for all data: 0.34902 with corrections 0.19711 Final wR= 0.20292 Final frame scales: Min= 0.4767 Max= 1.7648 Final absorption correction factors: Amin= 0.5214 Amax= 1.5041 PROFFIT INFO: Inet (after scale3 abspack): min=-1880.3582 max=1548801.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=48.5112 max=27783.0078 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/103 3083 reflections read from tmp file 806 reflections are rejected (737 as outliers, 69 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 86 64 53 31 36 25 24 22 65 Initial Chi^2= 2.50973 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.82740 Current error model SIG(F2)^2 = 538.60*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 445.64*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 445.64*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1548801- 119772 308 383608.83 31.45 100.00 117480- 4131 308 27011.23 6.71 82.47 4128- 2028 308 2738.10 2.62 28.90 2025- 1146 308 1565.61 1.97 16.23 1146- 758 308 927.71 1.28 0.97 757- 490 308 619.11 1.12 0.32 489- 303 308 393.58 0.99 0.65 303- 149 308 222.92 0.80 0.97 148- 16 308 76.83 0.48 0.00 16- -1880 311 -163.68 -0.34 0.00 ------------------------------------------------------------------------------------ 1548801- -1880 3083 41659.29 4.70 23.03 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 308 105008.90 10.76 52.92 1.59- 1.22 308 83890.77 8.42 41.56 1.22- 1.02 308 60057.26 6.25 28.90 1.02- 0.89 308 32901.59 3.80 17.53 0.89- 0.81 308 26932.58 3.35 13.31 0.80- 0.73 308 42599.40 4.65 24.03 0.73- 0.66 308 21790.00 2.93 12.34 0.66- 0.61 308 16606.88 2.42 12.66 0.61- 0.56 308 16779.95 2.52 15.58 0.56- 0.44 311 10330.68 1.95 11.58 ------------------------------------------------------------------------------------ 6.55- 0.44 3083 41659.29 4.70 23.03 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 308 105008.90 10.76 52.92 6.55- 1.22 616 94449.84 9.59 47.24 6.55- 1.02 924 82985.64 8.47 41.13 6.55- 0.89 1232 70464.63 7.31 35.23 6.55- 0.81 1540 61758.22 6.52 30.84 6.55- 0.73 1848 58565.08 6.21 29.71 6.55- 0.66 2156 53311.50 5.74 27.23 6.55- 0.61 2464 48723.42 5.32 25.41 6.55- 0.56 2772 45174.15 5.01 24.31 6.55- 0.44 3083 41659.29 4.70 23.03 ------------------------------------------------------------------------------------ 6.55- 0.44 3083 41659.29 4.70 23.03 Scale applied to data: s=0.645660 (maximum obs:1548801.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.197; Rsigma 0.050: data 3083 -> merged 482 With outlier rejection... Rint 0.173; Rsigma 0.052: data 3007 -> merged 482 Rejected total: 76, method kkm 63, method Blessing 13 Completeness direct cell (a, b, c) = (6.561, 6.561, 6.561), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445373, 6.560751 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.59 22 22 15.05 100.00 331 1.55 - 1.22 22 22 13.59 100.00 299 1.20 - 1.02 22 22 12.36 100.00 272 1.02 - 0.92 22 22 10.59 100.00 233 0.92 - 0.84 22 22 10.32 100.00 227 0.84 - 0.79 22 22 8.32 100.00 183 0.79 - 0.75 22 22 8.73 100.00 192 0.75 - 0.71 22 22 6.91 100.00 152 0.71 - 0.69 22 22 7.14 100.00 157 0.68 - 0.65 26 29 6.73 89.66 175 --------------------------------------------------------------- 7.37 - 0.65 224 227 9.92 98.68 2221 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:19:27 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.368317 7.362587 7.372194 120.2018 120.0561 89.7153 3007 Reflections read from file xs2212a.hkl 3007 Reflections used for space-group determination (up to diffraction limit of 0.45A); mean (I/sigma) = 4.50 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1516 1511 1515 1502 2271 2000 2003 3007 N (int>3sigma) = 0 167 176 235 165 289 450 463 672 Mean intensity = 0.0 0.8 0.8 1.2 0.8 1.0 23.4 25.7 25.0 Mean int/sigma = 0.0 1.4 1.4 1.9 1.3 1.6 4.3 4.7 4.5 Lattice type: P chosen Volume: 282.40 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.363 7.364 119.91 90.11 119.83 Niggli form: a.a = 53.948 b.b = 54.208 c.c = 54.229 b.c = -27.035 a.c = -0.108 a.b = -26.903 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.259 CUBIC F-lattice R(int) = 0.228 [ 2770] Vol = 1129.6 Cell: 10.390 10.442 10.411 90.01 89.85 90.04 Volume: 1129.59 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.258 RHOMBOHEDRAL R-lattice R(int) = 0.208 [ 2342] Vol = 847.2 Cell: 7.363 7.345 18.060 89.92 90.18 119.83 Volume: 847.19 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.258 RHOMBOHEDRAL R-lattice R(int) = 0.196 [ 746] Vol = 847.2 Trigonal Cell: 7.363 7.345 18.060 89.92 90.18 119.83 Volume: 847.19 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.378 TETRAGONAL I-lattice R(int) = 0.218 [ 2388] Vol = 564.8 Cell: 7.372 7.373 10.390 89.86 89.93 90.17 Volume: 564.79 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.447 TETRAGONAL I-lattice R(int) = 0.218 [ 2388] Vol = 564.8 Cell: 7.372 7.373 10.390 89.86 89.93 90.17 Volume: 564.79 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.407 ORTHORHOMBIC I-lattice R(int) = 0.166 [ 2313] Vol = 564.8 Cell: 7.372 10.390 7.373 89.86 89.83 90.07 Volume: 564.79 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.270 MONOCLINIC I-lattice R(int) = 0.164 [ 1810] Vol = 564.8 Cell: 10.390 7.372 7.373 90.17 90.14 90.07 Volume: 564.79 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.129 MONOCLINIC I-lattice R(int) = 0.158 [ 1793] Vol = 564.8 Cell: 7.364 7.345 10.442 89.97 90.04 89.89 Volume: 564.79 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.088 MONOCLINIC C-lattice R(int) = 0.176 [ 1833] Vol = 564.8 Cell: 10.390 10.442 7.345 89.97 134.87 90.04 Volume: 564.79 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) = 0.100 [ 895] Vol = 282.4 Cell: 7.345 7.363 7.364 119.91 90.11 119.83 Volume: 282.40 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1515 0 2003 1994 3007 N (int>3sigma) = 0 0 0 0 235 0 463 460 672 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 25.7 25.7 25.0 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.7 4.5 4.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.838 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 223 576 N I>3s 0 0 1 137 0.0 0.0 -0.0 1.7 0.5 0.5 0.1 2.5 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 0.228 2575 Fd-3m 1 1 227 C N N N N 37 2284 0.229 2638 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.390412 10.442170 10.411146 90.0089 89.8512 90.0446 ZERR 1.00 0.006008 0.001006 0.011022 0.1074 0.0024 0.0038 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 946776- 102027 336 310 48 6.5 351558.23 29.55 0.155 0.151 98632- 2629 401 387 48 8.1 12959.57 4.41 0.304 0.161 2593- 1492 488 479 48 10.0 2068.58 2.03 0.852 0.926 1483- 1002 484 477 48 9.9 1173.85 1.37 0.788 0.864 1001- 765 308 305 48 6.4 857.15 1.12 0.640 0.688 755- 568 306 299 48 6.2 618.06 0.91 0.679 0.752 566- 442 234 231 48 4.8 480.85 0.85 0.609 0.702 442- 296 207 203 48 4.2 360.63 0.70 0.731 0.839 295- 153 172 170 48 3.5 216.85 0.49 0.780 1.110 147- -310 147 146 50 2.9 38.38 0.14 0.965 2.475 ------------------------------------------------------------------------------------------- 946776- -310 3083 3007 482 6.2 38650.54 4.50 0.173 0.164 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-1.14 721 702 49 14.3 77528.96 8.37 0.177 0.170 0.028 1.13-0.89 532 521 48 10.9 44129.12 4.81 0.169 0.160 0.052 0.89-0.76 468 457 51 9.0 34910.92 4.01 0.179 0.175 0.069 0.76-0.69 359 353 48 7.4 28430.65 3.50 0.171 0.184 0.074 0.69-0.63 315 307 51 6.0 18202.86 2.59 0.174 0.168 0.099 0.63-0.58 247 236 50 4.7 10379.38 1.90 0.164 0.155 0.127 0.58-0.54 171 163 49 3.3 17067.97 2.64 0.150 0.135 0.108 0.54-0.52 118 117 48 2.4 4421.82 1.17 0.131 0.133 0.194 0.52-0.49 97 96 49 2.0 13014.73 2.38 0.072 0.074 0.113 0.48-0.45 55 55 39 1.4 4156.33 1.13 0.545 0.605 0.191 ------------------------------------------------------------------------------------------------------ inf-0.45 3083 3007 482 6.2 38650.54 4.50 0.173 0.164 0.052 inf-0.65 2275 2221 224 9.9 47434.52 5.31 0.174 0.168 0.046 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-1.14 702 49 49 100.0 14.3 77528.96 28.09 0.177 0.010 1.13-0.89 521 48 48 100.0 10.9 44129.12 13.98 0.169 0.023 0.89-0.76 457 51 51 100.0 9.0 34910.92 11.77 0.179 0.033 0.76-0.69 353 48 48 100.0 7.4 28430.65 9.46 0.171 0.032 0.69-0.63 307 54 51 94.4 6.0 18202.86 6.51 0.174 0.054 0.63-0.58 236 58 50 86.2 4.7 10379.38 3.94 0.164 0.064 0.58-0.54 163 55 49 89.1 3.3 17067.97 4.87 0.150 0.062 0.54-0.52 117 67 48 71.6 2.4 4421.82 1.90 0.131 0.120 0.52-0.49 96 83 49 59.0 2.0 13014.73 3.52 0.072 0.077 0.48-0.45 55 136 39 28.7 1.4 4156.33 1.33 0.545 0.946 -------------------------------------------------------------------------------------------- inf-0.45 3007 651 482 74.0 6.2 38650.54 13.33 0.173 0.029 inf-0.65 2221 227 224 98.7 9.9 47434.52 16.46 0.174 0.020 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.066415 0.012876 -0.008760 ( 0.000013 0.000014 0.000014 ) 0.014415 0.065207 -0.013263 ( 0.000012 0.000013 0.000013 ) 0.006057 -0.014659 -0.066262 ( 0.000016 0.000017 0.000017 ) M - matrix: 0.004655 -0.000004 -0.000011 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004633 -0.000006 ( 0.000001 0.000002 0.000002 ) -0.000011 -0.000006 0.004643 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.066415 0.012876 -0.008760 ( 0.000013 0.000014 0.000014 ) 0.014415 0.065207 -0.013263 ( 0.000012 0.000013 0.000013 ) 0.006057 -0.014659 -0.066262 ( 0.000016 0.000017 0.000017 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) unit cell: 10.396(2) 10.421(2) 10.409(2) 89.922(18) 89.868(17) 89.951(17) V = 1127.7(4) unit cell: 10.4087(5) 10.4087(5) 10.4087(5) 90.0 90.0 90.0 V = 1127.68(10) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.143) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-560.0000 max=7943967.0000 PROFFIT INFO: signal sum lp corr: min=-576.8383 max=1106771.8949 PROFFIT INFO: background sum: min=160.0000 max=7577.0000 PROFFIT INFO: background sum sig2: min=441.0000 max=5482.0000 PROFFIT INFO: num of signal pixels: min=43 max=485 PROFFIT INFO: Inet: min=-922.9413 max=1770835.0000 PROFFIT INFO: sig(Inet): min=57.2785 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.68 max=197.75 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 546 2118 3164 3836 4128 4788 5196 5432 5838 6098 6166 Percent 8.9 34.3 51.3 62.2 66.9 77.7 84.3 88.1 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3083 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 3083 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1770835- 132485 308 411481.60 77.66 100.00 132366- 4113 308 30831.21 19.97 100.00 4103- 2134 308 2936.11 7.30 98.70 2129- 1256 308 1633.60 3.87 52.92 1255- 834 308 1021.70 2.24 12.01 834- 555 308 688.58 1.68 7.14 555- 331 308 438.34 1.27 5.84 331- 156 308 242.33 0.73 1.62 156- 19 308 83.96 0.29 0.00 18- -923 311 -142.02 -0.27 0.00 ------------------------------------------------------------------------------------ 1770835- -923 3083 44877.69 11.46 37.79 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 308 110372.28 14.83 67.86 1.64- 1.26 308 84766.63 21.86 59.74 1.26- 1.09 308 59283.22 18.45 65.91 1.09- 0.96 308 54785.35 14.81 33.77 0.96- 0.88 308 16062.40 6.83 41.88 0.88- 0.81 308 53874.05 14.93 38.31 0.81- 0.76 308 19440.17 5.99 19.16 0.76- 0.71 308 23261.64 7.46 18.83 0.71- 0.67 308 23696.70 7.77 27.27 0.67- 0.63 311 3636.17 1.81 5.47 ------------------------------------------------------------------------------------ 6.00- 0.63 3083 44877.69 11.46 37.79 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:19:28 2019 Sorting 3083 observations 43 unique observations with > 7.00 F2/sig(F2) 3083 observations in 3 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 Total number of frames 307 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3083 observations in 3 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 Total number of frames 39 745 observations > 7.00 F2/sig(F2) 745 observations in 3 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 Total number of frames 39 Removing 'redundancy=1' reflections Average redundancy: 14.8 (Out of 745 removed 3 = 742, unique = 50) 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 742 observations in 3 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 Total number of frames 39 50 unique data precomputed (should be 50) 50 unique data with 742 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 14.8 (Out of 742 removed 0 = 742, unique = 50) 50 unique data precomputed (should be 50) 50 unique data with 742 observations RMS deviation of equivalent data = 0.22503 Rint = 0.17457 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.16969, wR= 0.21764 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07306, wR= 0.10631, Acormin=0.614, Acormax=1.312, Acor_av=0.989 F test: Probability=1.000, F= 5.355 Trying model 2 (ne=2, no=1)... Results: Rint= 0.06776, wR= 0.10029, Acormin=0.567, Acormax=1.352, Acor_av=0.974 F test: Probability=0.972, F= 1.158 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06544, wR= 0.09712, Acormin=0.587, Acormax=1.404, Acor_av=0.973 F test: Probability=0.785, F= 1.063 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06166, wR= 0.09220, Acormin=0.581, Acormax=1.434, Acor_av=0.964 F test: Probability=0.989, F= 1.191 Trying model 5 (ne=4, no=3)... Results: Rint= 0.05694, wR= 0.08883, Acormin=0.563, Acormax=1.405, Acor_av=0.952 F test: Probability=0.973, F= 1.160 Final absorption model (ne=4, no=3): Rint= 0.05694, Acormin=0.563, Acormax=1.405, Acor_av=0.952 Combined refinement in use Rint: 0.17673 There are 39 active scales (one needs to be fixed) Refinement control: frame scale #34 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 62 pars with 1953 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.22503 Using Levenberg-Marquardt: 0.00010 New wR= 0.09765 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17457 with corrections 0.06339 Rint for all data: 0.17673 with corrections 0.06634 3 observations identified as outliers and rejected Cycle 2 wR= 0.08056 Using Levenberg-Marquardt: 0.00001 New wR= 0.06914 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16969 with corrections 0.04378 Rint for all data: 0.17673 with corrections 0.05206 1 observations identified as outliers and rejected Cycle 3 wR= 0.06253 Using Levenberg-Marquardt: 0.00000 New wR= 0.06233 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16904 with corrections 0.04211 Rint for all data: 0.17673 with corrections 0.05202 1 observations identified as outliers and rejected Cycle 4 wR= 0.06005 Using Levenberg-Marquardt: 0.00000 New wR= 0.05991 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16900 with corrections 0.04169 Rint for all data: 0.17673 with corrections 0.05177 1 observations identified as outliers and rejected Cycle 5 wR= 0.05821 Using Levenberg-Marquardt: 0.00000 New wR= 0.05795 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.16838 with corrections 0.04114 Rint for all data: 0.17673 with corrections 0.05233 0 observations identified as outliers and rejected Final wR= 0.05795 Final frame scales: Min= 0.8561 Max= 1.2391 Final absorption correction factors: Amin= 0.5586 Amax= 1.3487 PROFFIT INFO: Inet (after scale3 abspack): min=-933.3495 max=1244226.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=49.5883 max=24683.8730 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/103 3083 reflections read from tmp file 109 reflections are rejected (108 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 7 4 2 4 2 3 127 Initial Chi^2= 0.51602 Cycle 1, Chi^2= 1.01530 Current error model SIG(F2)^2 = 63.24*I_RAW + 10.99*I_BACK+(0.03726*)^2 Cycle 2, Chi^2= 1.02124 Current error model SIG(F2)^2 = 82.62*I_RAW + 6.89*I_BACK+(0.02710*)^2 Cycle 3, Chi^2= 1.01732 Current error model SIG(F2)^2 = 94.84*I_RAW + 4.82*I_BACK+(0.02196*)^2 Cycle 4, Chi^2= 1.00991 Current error model SIG(F2)^2 = 101.36*I_RAW + 3.90*I_BACK+(0.01983*)^2 Cycle 5, Chi^2= 1.00377 Current error model SIG(F2)^2 = 104.02*I_RAW + 3.59*I_BACK+(0.01920*)^2 Cycle 6, Chi^2= 1.00110 Current error model SIG(F2)^2 = 104.88*I_RAW + 3.51*I_BACK+(0.01904*)^2 Cycle 7, Chi^2= 1.00029 Current error model SIG(F2)^2 = 105.11*I_RAW + 3.48*I_BACK+(0.01901*)^2 Cycle 8, Chi^2= 1.00007 Current error model SIG(F2)^2 = 105.17*I_RAW + 3.48*I_BACK+(0.01900*)^2 Final Chi^2= 1.00007 Final error model SIG(F2)^2 = 105.17*I_RAW + 3.48*I_BACK+(0.01900*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1244226- 125881 308 394228.42 36.58 100.00 125579- 3754 308 31513.77 12.78 100.00 3753- 2105 308 2843.49 5.65 98.70 2097- 1218 308 1579.97 3.72 56.49 1215- 826 308 991.90 2.52 14.94 825- 548 308 682.33 2.19 8.77 548- 329 308 432.60 1.89 8.77 329- 157 308 239.95 1.37 1.95 156- 17 308 83.02 0.77 0.32 16- -933 311 -144.19 -0.58 0.00 ------------------------------------------------------------------------------------ 1244226- -933 3083 43202.90 6.68 38.96 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 308 105235.66 11.19 70.13 1.64- 1.26 308 80830.36 10.46 60.39 1.26- 1.09 308 59079.05 8.90 67.86 1.09- 0.96 308 52240.89 7.36 34.42 0.96- 0.88 308 15477.52 4.68 44.48 0.88- 0.81 308 52259.43 8.37 39.61 0.81- 0.76 308 18655.99 3.99 18.83 0.76- 0.71 308 22116.84 5.11 18.83 0.71- 0.67 308 22957.06 5.19 29.22 0.67- 0.63 311 3562.35 1.63 6.11 ------------------------------------------------------------------------------------ 6.00- 0.63 3083 43202.90 6.68 38.96 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 308 105235.66 11.19 70.13 6.00- 1.26 616 93033.01 10.82 65.26 6.00- 1.09 924 81715.02 10.18 66.13 6.00- 0.96 1232 74346.49 9.48 58.20 6.00- 0.88 1540 62572.70 8.52 55.45 6.00- 0.81 1848 60853.82 8.49 52.81 6.00- 0.76 2156 54825.56 7.85 47.96 6.00- 0.71 2464 50736.97 7.51 44.32 6.00- 0.67 2772 47650.31 7.25 42.64 6.00- 0.63 3083 43202.90 6.68 38.96 ------------------------------------------------------------------------------------ 6.00- 0.63 3083 43202.90 6.68 38.96 Scale applied to data: s=0.803712 (maximum obs:1244226.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.052; Rsigma 0.033: data 3083 -> merged 162 With outlier rejection... Rint 0.041; Rsigma 0.033: data 3067 -> merged 162 Rejected total: 16, method kkm 12, method Blessing 4 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626529, 6.009454 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.37 - 1.76 14 14 19.71 100.00 276 1.73 - 1.27 14 14 22.57 100.00 316 1.26 - 1.06 14 14 24.79 100.00 347 1.05 - 0.97 14 14 21.71 100.00 304 0.95 - 0.88 14 14 22.79 100.00 319 0.87 - 0.81 14 14 20.00 100.00 280 0.80 - 0.76 14 14 21.21 100.00 297 0.76 - 0.72 14 14 17.79 100.00 249 0.72 - 0.69 14 14 18.93 100.00 265 0.69 - 0.65 19 19 16.42 100.00 312 --------------------------------------------------------------- 7.37 - 0.65 145 145 20.45 100.00 2965 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:19:27 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.368317 7.362587 7.372194 120.2018 120.0561 89.7153 3007 Reflections read from file xs2212a.hkl 3007 Reflections used for space-group determination (up to diffraction limit of 0.45A); mean (I/sigma) = 4.50 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1516 1511 1515 1502 2271 2000 2003 3007 N (int>3sigma) = 0 167 176 235 165 289 450 463 672 Mean intensity = 0.0 0.8 0.8 1.2 0.8 1.0 23.4 25.7 25.0 Mean int/sigma = 0.0 1.4 1.4 1.9 1.3 1.6 4.3 4.7 4.5 Lattice type: P chosen Volume: 282.40 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.363 7.364 119.91 90.11 119.83 Niggli form: a.a = 53.948 b.b = 54.208 c.c = 54.229 b.c = -27.035 a.c = -0.108 a.b = -26.903 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.259 CUBIC F-lattice R(int) = 0.228 [ 2770] Vol = 1129.6 Cell: 10.390 10.442 10.411 90.01 89.85 90.04 Volume: 1129.59 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.258 RHOMBOHEDRAL R-lattice R(int) = 0.208 [ 2342] Vol = 847.2 Cell: 7.363 7.345 18.060 89.92 90.18 119.83 Volume: 847.19 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.258 RHOMBOHEDRAL R-lattice R(int) = 0.196 [ 746] Vol = 847.2 Trigonal Cell: 7.363 7.345 18.060 89.92 90.18 119.83 Volume: 847.19 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.378 TETRAGONAL I-lattice R(int) = 0.218 [ 2388] Vol = 564.8 Cell: 7.372 7.373 10.390 89.86 89.93 90.17 Volume: 564.79 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.447 TETRAGONAL I-lattice R(int) = 0.218 [ 2388] Vol = 564.8 Cell: 7.372 7.373 10.390 89.86 89.93 90.17 Volume: 564.79 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.407 ORTHORHOMBIC I-lattice R(int) = 0.166 [ 2313] Vol = 564.8 Cell: 7.372 10.390 7.373 89.86 89.83 90.07 Volume: 564.79 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.270 MONOCLINIC I-lattice R(int) = 0.164 [ 1810] Vol = 564.8 Cell: 10.390 7.372 7.373 90.17 90.14 90.07 Volume: 564.79 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.129 MONOCLINIC I-lattice R(int) = 0.158 [ 1793] Vol = 564.8 Cell: 7.364 7.345 10.442 89.97 90.04 89.89 Volume: 564.79 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.088 MONOCLINIC C-lattice R(int) = 0.176 [ 1833] Vol = 564.8 Cell: 10.390 10.442 7.345 89.97 134.87 90.04 Volume: 564.79 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) = 0.100 [ 895] Vol = 282.4 Cell: 7.345 7.363 7.364 119.91 90.11 119.83 Volume: 282.40 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1515 0 2003 1994 3007 N (int>3sigma) = 0 0 0 0 235 0 463 460 672 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 25.7 25.7 25.0 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.7 4.5 4.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.838 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 223 576 N I>3s 0 0 1 137 0.0 0.0 -0.0 1.7 0.5 0.5 0.1 2.5 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 0.228 2575 Fd-3m 1 1 227 C N N N N 37 2284 0.229 2638 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.390412 10.442170 10.411146 90.0089 89.8512 90.0446 ZERR 1.00 0.006008 0.001006 0.011022 0.1074 0.0024 0.0038 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1143849- 102126 376 365 27 13.5 343069.07 33.77 0.036 0.044 76263- 1746 579 576 27 21.3 5521.63 7.87 0.097 0.127 1744- 793 602 601 27 22.3 1199.08 2.80 0.221 0.279 770- 351 587 587 27 21.7 537.00 1.88 0.380 0.531 348- 67 486 486 27 18.0 230.36 1.20 0.549 0.836 63- -154 453 452 27 16.7 0.57 0.14 0.964 4.071 ------------------------------------------------------------------------------------------- 1143849- -154 3083 3067 162 18.9 42239.57 6.62 0.041 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-1.27 594 590 27 21.9 92937.15 11.04 0.030 0.036 0.023 1.26-0.97 654 651 28 23.3 52005.76 7.67 0.037 0.050 0.029 0.95-0.81 588 585 27 21.7 35189.05 6.77 0.042 0.046 0.040 0.81-0.73 534 531 27 19.7 15093.11 3.68 0.062 0.073 0.057 0.73-0.67 480 478 28 17.1 23483.07 5.11 0.079 0.099 0.059 0.66-0.63 233 232 25 9.3 4461.81 1.81 0.150 0.104 0.123 ------------------------------------------------------------------------------------------------------ inf-0.63 3083 3067 162 18.9 42239.57 6.62 0.041 0.049 0.033 inf-0.65 2978 2963 144 20.6 43469.97 6.77 0.040 0.047 0.033 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-1.27 590 27 27 100.0 21.9 92937.15 48.37 0.030 0.007 1.26-0.97 651 28 28 100.0 23.3 52005.76 34.67 0.037 0.008 0.95-0.81 585 27 27 100.0 21.7 35189.05 31.79 0.042 0.011 0.81-0.73 531 27 27 100.0 19.7 15093.11 15.22 0.062 0.016 0.73-0.67 478 28 28 100.0 17.1 23483.07 22.31 0.079 0.015 0.66-0.63 232 25 25 100.0 9.3 4461.81 5.75 0.150 0.043 -------------------------------------------------------------------------------------------- inf-0.63 3067 162 162 100.0 18.9 42239.57 29.27 0.041 0.010 inf-0.65 2963 144 144 100.0 20.6 43469.97 30.13 0.040 0.009 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:25:34 2019) ID: 3668; threads 40; handles 811; mem 515316.00 (1204688.00)kB; time: 1w 4d 23h 36m 22s MEMORY INFO: Memory PF:272.0, Ph:634.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.2,peak PF: 700.2, WS: 471.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:274.0, Ph:636.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.0,peak PF: 700.2, WS: 473.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:25:34 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000094 0.000066 0.000095 ) 0.064809 0.092374 0.027273 ( 0.000110 0.000077 0.000110 ) 0.045523 0.057900 0.132205 ( 0.000132 0.000092 0.000133 ) 7.38096 ( 0.00713 ) 7.36649 ( 0.00761 ) 7.42630 ( 0.00879 ) 120.52449 ( 0.11792 ) 120.40327 ( 0.11410 ) 89.27095 ( 0.08099 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:25:35 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000094 0.000066 0.000095 ) 0.064809 0.092374 0.027273 ( 0.000110 0.000077 0.000110 ) 0.045523 0.057900 0.132205 ( 0.000132 0.000092 0.000133 ) M - matrix: 0.013795 0.004556 0.009167 ( 0.000025 0.000016 0.000022 ) 0.004556 0.013994 0.009349 ( 0.000016 0.000019 0.000018 ) 0.009167 0.009349 0.018509 ( 0.000022 0.000018 0.000036 ) unit cell: 7.381(7) 7.366(8) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.82 | 24 | 1.005 ( 0.047) | 1.008 ( 0.130) | 0.907 ( 0.354) | 0.79- 0.69 | 24 | 0.998 ( 0.044) | 1.006 ( 0.137) | 1.289 ( 0.497) | 0.69- 0.63 | 23 | 0.979 ( 0.051) | 0.913 ( 0.103) | 1.157 ( 0.432) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.510) | 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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb PROFFITPEAK info: 105 peaks in the peak location table UB fit with 7 obs out of 56 (total:56,skipped:0) (12.50%) UB - matrix: 0.085246 -0.045663 0.016794 ( 0.000934 0.000252 0.000442 ) 0.063905 0.092403 0.027090 ( 0.001923 0.000520 0.000909 ) 0.044724 0.056701 0.132070 ( 0.004936 0.001334 0.002334 ) M - matrix: 0.013351 0.004548 0.009070 ( 0.000530 0.000342 0.000666 ) 0.004548 0.013838 0.009225 ( 0.000342 0.000181 0.000237 ) 0.009070 0.009225 0.018458 ( 0.000666 0.000237 0.000619 ) unit cell: 7.52(10) 7.38(9) 7.38(17) 120(2) 120(3) 90(1) V = 290(8) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 4, #refl in peak table: 56 #indexed refl 54, indexation with best UB: 96.4286% Lattice: 7.3776 7.3640 7.3570 119.903 119.944 90.203 282.780 Rotation: -22.595 24.713 -35.273 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 56 obs out of 56 (total:56,skipped:0) (100.00%) UB - matrix: 0.088048 -0.044233 0.012686 ( 0.000326 0.000135 0.000151 ) 0.062280 0.094364 0.026300 ( 0.000229 0.000095 0.000106 ) 0.049624 0.055454 0.133192 ( 0.000179 0.000074 0.000083 ) M - matrix: 0.014094 0.004734 0.009365 ( 0.000066 0.000031 0.000029 ) 0.004734 0.013936 0.009307 ( 0.000031 0.000023 0.000017 ) 0.009365 0.009307 0.018593 ( 0.000029 0.000017 0.000023 ) unit cell: 7.325(19) 7.364(14) 7.357(8) 119.90(15) 119.93(18) 90.29(18) V = 280.6(10) OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 UB - matrix: 0.088071 -0.044207 0.012724 ( 0.000327 0.000135 0.000152 ) 0.062261 0.094375 0.026274 ( 0.000227 0.000094 0.000105 ) 0.049612 0.055450 0.133163 ( 0.000179 0.000074 0.000083 ) M - matrix: 0.014094 0.004733 0.009363 ( 0.000067 0.000031 0.000029 ) 0.004733 0.013936 0.009301 ( 0.000031 0.000023 0.000016 ) 0.009363 0.009301 0.018585 ( 0.000029 0.000016 0.000023 ) UB fit with 56 obs out of 56 (total:56,skipped:0) (100.00%) unit cell: 7.325(19) 7.363(14) 7.357(8) 119.89(15) 119.94(18) 90.29(18) V = 280.6(10) UB fit with 56 obs out of 56 (total:56,skipped:0) (100.00%) UB - matrix: 0.088071 -0.044207 0.012724 ( 0.000327 0.000135 0.000152 ) 0.062261 0.094375 0.026274 ( 0.000227 0.000094 0.000105 ) 0.049612 0.055450 0.133163 ( 0.000179 0.000074 0.000083 ) M - matrix: 0.014094 0.004733 0.009363 ( 0.000067 0.000031 0.000029 ) 0.004733 0.013936 0.009301 ( 0.000031 0.000023 0.000016 ) 0.009363 0.009301 0.018585 ( 0.000029 0.000016 0.000023 ) unit cell: 7.325(19) 7.363(14) 7.357(8) 119.89(15) 119.94(18) 90.29(18) V = 280.6(10) OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 OTKP changes: 23 1 1 1 UB - matrix: 0.088071 -0.044207 0.012724 ( 0.000327 0.000135 0.000152 ) 0.062261 0.094375 0.026274 ( 0.000227 0.000094 0.000105 ) 0.049612 0.055450 0.133163 ( 0.000179 0.000074 0.000083 ) M - matrix: 0.014094 0.004733 0.009363 ( 0.000067 0.000031 0.000029 ) 0.004733 0.013936 0.009301 ( 0.000031 0.000023 0.000016 ) 0.009363 0.009301 0.018585 ( 0.000029 0.000016 0.000023 ) UB fit with 56 obs out of 56 (total:56,skipped:0) (100.00%) unit cell: 7.325(19) 7.363(14) 7.357(8) 119.89(15) 119.94(18) 90.29(18) V = 280.6(10) 56 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Run 4 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 466 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 56 obs out of 56 (total:56,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb 0 of 49 peaks identified as outliers and rejected 49 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 49 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 49 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.59 | 5 | 0.898 ( 0.095) | 0.938 ( 0.109) | 1.251 ( 0.591) | 2.36- 1.99 | 5 | 0.914 ( 0.084) | 0.935 ( 0.111) | 0.805 ( 0.182) | 1.83- 1.57 | 5 | 0.904 ( 0.108) | 0.901 ( 0.140) | 0.941 ( 0.448) | 1.56- 1.35 | 5 | 1.001 ( 0.039) | 1.057 ( 0.073) | 0.780 ( 0.477) | 1.35- 1.06 | 5 | 0.959 ( 0.073) | 0.972 ( 0.090) | 0.981 ( 0.424) | 1.00- 0.89 | 5 | 0.999 ( 0.054) | 1.011 ( 0.081) | 0.948 ( 0.281) | 0.88- 0.86 | 5 | 1.016 ( 0.014) | 1.021 ( 0.042) | 1.091 ( 0.405) | 0.86- 0.75 | 5 | 0.999 ( 0.037) | 1.045 ( 0.112) | 1.052 ( 0.310) | 0.72- 0.68 | 5 | 0.972 ( 0.046) | 0.950 ( 0.049) | 1.096 ( 0.224) | 0.68- 0.63 | 4 | 0.968 ( 0.050) | 0.902 ( 0.054) | 1.271 ( 0.263) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.63 | 49 | 0.963 ( 0.078) | 0.975 ( 0.107) | 1.016 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 49 obs out of 49 (total:49,skipped:0) (100.00%) UB - matrix: 0.088249 -0.044148 0.013035 ( 0.000207 0.000082 0.000088 ) 0.061549 0.094460 0.026039 ( 0.000146 0.000058 0.000062 ) 0.049344 0.055428 0.133158 ( 0.000097 0.000038 0.000041 ) M - matrix: 0.014011 0.004653 0.009324 ( 0.000042 0.000019 0.000016 ) 0.004653 0.013944 0.009265 ( 0.000019 0.000014 0.000009 ) 0.009324 0.009265 0.018579 ( 0.000016 0.000009 0.000012 ) unit cell: 7.342(12) 7.346(9) 7.353(4) 119.87(9) 120.06(11) 90.02(11) V = 280.7(6) OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 UB - matrix: 0.088019 -0.044262 0.012833 ( 0.000175 0.000070 0.000075 ) 0.061836 0.094392 0.026271 ( 0.000113 0.000045 0.000048 ) 0.049298 0.055440 0.133142 ( 0.000099 0.000039 0.000042 ) M - matrix: 0.014001 0.004674 0.009318 ( 0.000035 0.000016 0.000016 ) 0.004674 0.013943 0.009293 ( 0.000016 0.000011 0.000008 ) 0.009318 0.009293 0.018582 ( 0.000016 0.000008 0.000012 ) UB fit with 49 obs out of 49 (total:49,skipped:0) (100.00%) unit cell: 7.344(10) 7.357(7) 7.358(4) 119.96(8) 119.98(9) 90.09(9) V = 281.1(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 463 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 49 obs out of 49 (total:49,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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb 0 of 51 peaks identified as outliers and rejected 51 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 51 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 51 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 2.99 | 5 | 0.855 ( 0.110) | 0.867 ( 0.136) | 1.296 ( 0.563) | 2.59- 2.11 | 5 | 0.899 ( 0.071) | 0.925 ( 0.103) | 0.823 ( 0.200) | 2.00- 1.59 | 5 | 0.939 ( 0.090) | 0.980 ( 0.108) | 1.042 ( 0.398) | 1.59- 1.45 | 5 | 0.950 ( 0.098) | 0.963 ( 0.150) | 0.880 ( 0.437) | 1.45- 1.19 | 5 | 0.967 ( 0.071) | 1.004 ( 0.074) | 0.874 ( 0.493) | 1.14- 1.00 | 5 | 1.001 ( 0.059) | 0.999 ( 0.102) | 0.933 ( 0.298) | 1.00- 0.88 | 5 | 1.024 ( 0.033) | 1.057 ( 0.053) | 0.978 ( 0.298) | 0.88- 0.79 | 5 | 1.015 ( 0.025) | 1.072 ( 0.105) | 1.002 ( 0.428) | 0.79- 0.69 | 5 | 0.973 ( 0.046) | 0.975 ( 0.041) | 1.145 ( 0.259) | 0.69- 0.63 | 6 | 0.967 ( 0.042) | 0.902 ( 0.046) | 1.199 ( 0.266) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 0.63 | 51 | 0.959 ( 0.085) | 0.973 ( 0.115) | 1.021 ( 0.406) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 76 | 0.979 ( 0.036) | 1.027 ( 0.074) | 1.142 ( 0.510) | 10.3-14.9 | 76 | 0.980 ( 0.043) | 1.038 ( 0.071) | 1.215 ( 0.580) | 14.9-18.9 | 76 | 0.999 ( 0.239) | 1.024 ( 0.100) | 1.254 ( 1.224) | 19.0-23.5 | 76 | 0.955 ( 0.057) | 1.000 ( 0.083) | 0.935 ( 0.426) | 23.5-26.9 | 76 | 0.961 ( 0.061) | 0.996 ( 0.096) | 0.963 ( 0.436) | 27.0-32.2 | 76 | 0.943 ( 0.091) | 0.949 ( 0.114) | 0.932 ( 0.475) | 32.4-36.3 | 76 | 0.928 ( 0.173) | 0.918 ( 0.141) | 1.063 ( 0.668) | 36.3-38.7 | 76 | 0.876 ( 0.096) | 0.841 ( 0.126) | 1.011 ( 0.489) | 38.9-42.0 | 76 | 0.893 ( 0.093) | 0.847 ( 0.131) | 1.058 ( 0.494) | 42.0-50.1 | 72 | 0.881 ( 0.114) | 0.802 ( 0.131) | 0.984 ( 0.469) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 756 | 0.940 ( 0.124) | 0.945 ( 0.137) | 1.056 ( 0.630) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.13 e2 dimension: a=-0.0070 b=1.24 e3 dimension: a=-0.0001 b=1.10 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3812 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:25:46 2019 PROFFITMAIN - Started at Wed Aug 21 13:25:46 2019 OTKP changes: 311 2 3 4 OTKP changes: 311 2 3 4 OTKP changes: 311 2 3 4 UB - matrix: 0.087572 -0.046029 0.016788 ( 0.000090 0.000065 0.000090 ) 0.063414 0.092451 0.026844 ( 0.000103 0.000075 0.000104 ) 0.045283 0.057673 0.132020 ( 0.000105 0.000077 0.000106 ) M - matrix: 0.013741 0.004444 0.009151 ( 0.000023 0.000015 0.000018 ) 0.004444 0.013992 0.009323 ( 0.000015 0.000018 0.000016 ) 0.009151 0.009323 0.018432 ( 0.000018 0.000016 0.000029 ) UB fit with 360 obs out of 756 (total:756,skipped:0) (47.62%) unit cell: 7.397(7) 7.366(7) 7.431(7) 120.75(11) 120.28(10) 88.85(8) V = 284.6(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) UB - matrix: 0.087573 -0.046164 0.017210 ( 0.000107 0.000066 0.000100 ) 0.064609 0.092338 0.027106 ( 0.000091 0.000056 0.000085 ) 0.045824 0.057751 0.132077 ( 0.000107 0.000066 0.000100 ) M - matrix: 0.013943 0.004570 0.009311 ( 0.000024 0.000014 0.000018 ) 0.004570 0.013993 0.009336 ( 0.000014 0.000014 0.000014 ) 0.009311 0.009336 0.018475 ( 0.000018 0.000014 0.000027 ) unit cell: 7.375(7) 7.366(7) 7.437(7) 120.52(9) 120.47(10) 89.16(7) V = 283.5(4) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.150) HKL list info: 1285 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087480 -0.046159 0.017366 ( 0.000099 0.000062 0.000092 ) 0.064775 0.092369 0.027254 ( 0.000086 0.000053 0.000080 ) 0.045701 0.057837 0.132144 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013937 0.004588 0.009324 ( 0.000023 0.000013 0.000018 ) 0.004588 0.014008 0.009359 ( 0.000013 0.000014 0.000013 ) 0.009324 0.009359 0.018506 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.380(6) 7.366(6) 7.434(6) 120.52(9) 120.46(9) 89.22(7) V = 283.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 204 obs out of 212 (total:212,skipped:0) (96.23%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.118016 0.039028 0.078663 ( 0.000076 0.000047 0.000070 ) 0.000076 0.111559 0.056285 ( 0.000079 0.000050 0.000073 ) -0.000027 -0.000072 0.095401 ( 0.000090 0.000056 0.000083 ) M - matrix: 0.013928 0.004614 0.009285 ( 0.000018 0.000011 0.000014 ) 0.004614 0.013969 0.009342 ( 0.000011 0.000012 0.000011 ) 0.009285 0.009342 0.018457 ( 0.000014 0.000011 0.000021 ) UB fit with 207 obs out of 212 (total:212,skipped:0) (97.64%) unit cell: 7.373(5) 7.379(5) 7.431(8) 120.48(9) 120.25(9) 89.47(6) V = 284.0(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1304 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.087804 -0.044309 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094149 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055798 0.133161 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004658 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009312 0.018585 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3551(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1267 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 51 obs out of 51 (total:51,skipped:0) (100.00%) UB - matrix: 0.088079 -0.044261 0.012853 ( 0.000170 0.000069 0.000074 ) 0.061817 0.094410 0.026271 ( 0.000103 0.000042 0.000045 ) 0.049335 0.055434 0.133149 ( 0.000096 0.000040 0.000042 ) M - matrix: 0.014013 0.004672 0.009325 ( 0.000034 0.000015 0.000015 ) 0.004672 0.013945 0.009292 ( 0.000015 0.000011 0.000008 ) 0.009325 0.009292 0.018584 ( 0.000015 0.000008 0.000012 ) unit cell: 7.342(9) 7.356(7) 7.358(4) 119.95(7) 120.01(9) 90.06(9) V = 281.0(5) OTKP changes: 51 1 1 1 OTKP changes: 51 1 1 1 OTKP changes: 51 1 1 1 UB - matrix: 0.088065 -0.044270 0.012839 ( 0.000169 0.000069 0.000074 ) 0.061834 0.094405 0.026285 ( 0.000104 0.000043 0.000045 ) 0.049335 0.055434 0.133151 ( 0.000097 0.000040 0.000042 ) M - matrix: 0.014013 0.004674 0.009325 ( 0.000034 0.000015 0.000015 ) 0.004674 0.013945 0.009294 ( 0.000015 0.000011 0.000008 ) 0.009325 0.009294 0.018585 ( 0.000015 0.000008 0.000012 ) UB fit with 51 obs out of 51 (total:51,skipped:0) (100.00%) unit cell: 7.342(9) 7.356(7) 7.358(4) 119.96(7) 120.00(9) 90.06(9) V = 281.0(5) Run 4 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 447 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: 0.088065 -0.044270 0.012839 ( 0.000169 0.000069 0.000074 ) 0.061834 0.094405 0.026285 ( 0.000104 0.000043 0.000045 ) 0.049335 0.055434 0.133151 ( 0.000097 0.000040 0.000042 ) M - matrix: 0.014013 0.004674 0.009325 ( 0.000034 0.000015 0.000015 ) 0.004674 0.013945 0.009294 ( 0.000015 0.000011 0.000008 ) 0.009325 0.009294 0.018585 ( 0.000015 0.000008 0.000012 ) UB fit with 51 obs out of 51 (total:51,skipped:0) (100.00%) unit cell: 7.342(9) 7.356(7) 7.358(4) 119.96(7) 120.00(9) 90.06(9) V = 281.0(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 68.89 ph= 0.28 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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117766 0.038868 0.078516 ( 0.000039 0.000037 0.000044 ) 0.000051 0.111492 0.056133 ( 0.000028 0.000026 0.000031 ) -0.000083 -0.000149 0.096116 ( 0.000032 0.000030 0.000036 ) M - matrix: 0.013869 0.004583 0.009241 ( 0.000009 0.000006 0.000007 ) 0.004583 0.013941 0.009296 ( 0.000006 0.000007 0.000006 ) 0.009241 0.009296 0.018554 ( 0.000007 0.000006 0.000010 ) UB fit with 749 obs out of 756 (total:756,skipped:0) (99.07%) unit cell: 7.369(3) 7.362(2) 7.371(3) 120.19(4) 120.03(4) 89.71(3) V = 282.47(17) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 80 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof 3317 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:25:52 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.150) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-557.0000 max=7904045.0000 PROFFIT INFO: signal sum lp corr: min=-576.8383 max=1106313.4880 PROFFIT INFO: background sum: min=62.0000 max=7519.0000 PROFFIT INFO: background sum sig2: min=450.0000 max=5482.0000 PROFFIT INFO: num of signal pixels: min=44 max=485 PROFFIT INFO: Inet: min=-922.9413 max=1770101.6250 PROFFIT INFO: sig(Inet): min=57.2785 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.70 max=197.69 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 306 1148 1725 2077 2223 2587 2796 2927 3147 3281 3317 Percent 9.2 34.6 52.0 62.6 67.0 78.0 84.3 88.2 94.9 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3317 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 3317 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1770102- 129139 331 403021.25 76.37 100.00 129039- 4014 331 30261.57 19.90 100.00 4008- 2099 331 2886.87 7.09 98.79 2096- 1231 331 1595.70 3.82 50.45 1229- 819 331 1001.58 2.28 12.39 819- 534 331 675.76 1.66 6.65 533- 326 331 427.43 1.24 5.14 325- 150 331 235.46 0.70 1.21 150- 13 331 76.59 0.29 0.00 13- -923 338 -136.95 -0.27 0.00 ------------------------------------------------------------------------------------ 1770102- -923 3317 43911.37 11.28 37.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 331 100449.40 17.11 68.58 1.59- 1.22 331 85642.24 19.16 57.40 1.22- 1.02 331 58377.34 16.21 49.85 1.02- 0.89 331 35488.01 10.68 37.16 0.89- 0.79 331 31500.29 9.71 32.33 0.79- 0.72 331 42442.54 12.69 42.30 0.72- 0.66 331 25755.78 8.11 25.38 0.66- 0.61 331 25248.33 7.68 25.68 0.61- 0.55 331 22037.36 7.20 21.15 0.55- 0.44 338 12829.74 4.43 14.50 ------------------------------------------------------------------------------------ 6.55- 0.44 3317 43911.37 11.28 37.38 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:25:52 2019 Sorting 3317 observations 87 unique observations with > 7.00 F2/sig(F2) 3317 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 24 332 Total number of frames 332 Maximum number of 87 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 3317 observations in 4 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 25 78 4 0 6 85 Total number of frames 85 789 observations > 7.00 F2/sig(F2) 789 observations in 4 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 25 78 4 0 5 84 Total number of frames 84 Removing 'redundancy=1' reflections Average redundancy: 6.3 (Out of 789 removed 36 = 753, unique = 120) 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 753 observations in 4 runs Run # start # end # total # 1 0 25 26 2 0 25 52 3 0 25 78 4 0 5 84 Total number of frames 84 120 unique data precomputed (should be 120) 120 unique data with 753 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.3 (Out of 753 removed 0 = 753, unique = 120) 120 unique data precomputed (should be 120) 120 unique data with 753 observations RMS deviation of equivalent data = 0.38235 Rint = 0.33129 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.32929, wR= 0.45511 Trying model 1 (ne=2, no=0)... Results: Rint= 0.25636, wR= 0.35196, Acormin=0.536, Acormax=1.481, Acor_av=0.984 F test: Probability=1.000, F= 1.637 Trying model 2 (ne=2, no=1)... Results: Rint= 0.25654, wR= 0.35432, Acormin=0.442, Acormax=1.554, Acor_av=0.903 F test: Probability=0.000, F= 0.994 Trying model 3 (ne=4, no=0)... Results: Rint= 0.25331, wR= 0.34838, Acormin=0.528, Acormax=1.516, Acor_av=0.951 F test: Probability=0.547, F= 1.009 Trying model 4 (ne=4, no=1)... Results: Rint= 0.25641, wR= 0.35362, Acormin=0.337, Acormax=1.467, Acor_av=0.886 F test: Probability=0.000, F= 0.980 Trying model 5 (ne=4, no=3)... Results: Rint= 0.25332, wR= 0.34480, Acormin=0.255, Acormax=1.522, Acor_av=0.777 F test: Probability=0.000, F= 0.993 Trying model 6 (ne=6, no=0)... Results: Rint= 0.25564, wR= 0.33073, Acormin=0.224, Acormax=1.635, Acor_av=0.883 F test: Probability=0.000, F= 0.970 Trying model 7 (ne=6, no=1)... Results: Rint= 0.25635, wR= 0.33111, Acormin=0.110, Acormax=1.621, Acor_av=0.854 F test: Probability=0.000, F= 0.960 Trying model 8 (ne=6, no=3)... Results: Rint= 0.25781, wR= 0.32726, Acormin=0.050, Acormax=1.559, Acor_av=0.734 F test: Probability=0.000, F= 0.938 Trying model 9 (ne=6, no=5)... Results: Rint= 0.32224, wR= 0.39562, Acormin=-0.035, Acormax=2.256, Acor_av=0.414 F test: Probability=0.000, F= 0.589 Trying model 10 (ne=8, no=0)... Results: Rint= 0.25173, wR= 0.31099, Acormin=0.103, Acormax=1.779, Acor_av=0.847 F test: Probability=0.000, F= 0.973 Trying model 11 (ne=8, no=1)... Results: Rint= 0.31077, wR= 0.36664, Acormin=-0.119, Acormax=1.411, Acor_av=0.570 F test: Probability=0.000, F= 0.635 Trying model 12 (ne=8, no=3)... Results: Rint= 0.30926, wR= 0.36987, Acormin=-0.003, Acormax=0.094, Acor_av=0.040 F test: Probability=0.000, F= 0.633 Trying model 13 (ne=8, no=5)... Results: Rint= 0.27231, wR= 0.33185, Acormin=-0.005, Acormax=0.099, Acor_av=0.043 F test: Probability=0.000, F= 0.801 Trying model 14 (ne=8, no=7)... Results: Rint= 0.19135, wR= 0.25153, Acormin=0.004, Acormax=0.104, Acor_av=0.047 F test: Probability=1.000, F= 1.580 Final absorption model (ne=2, no=0): Rint= 0.25636, Acormin=0.536, Acormax=1.481, Acor_av=0.984 Combined refinement in use Rint: 0.34556 There are 84 active scales (one needs to be fixed) Refinement control: frame scale #27 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 88 pars with 3916 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.38235 Using Levenberg-Marquardt: 0.00010 New wR= 0.22567 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.33129 with corrections 0.19109 Rint for all data: 0.34556 with corrections 0.20699 0 observations identified as outliers and rejected Cycle 2 wR= 0.22567 Using Levenberg-Marquardt: 0.00001 New wR= 0.21523 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.33129 with corrections 0.18519 Rint for all data: 0.34556 with corrections 0.20120 0 observations identified as outliers and rejected Cycle 3 wR= 0.21523 Using Levenberg-Marquardt: 0.00000 New wR= 0.21324 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.33129 with corrections 0.18431 Rint for all data: 0.34556 with corrections 0.20030 0 observations identified as outliers and rejected Cycle 4 wR= 0.21324 Using Levenberg-Marquardt: 0.00000 New wR= 0.21430 Using Levenberg-Marquardt: 0.00000 New wR= 0.21430 Using Levenberg-Marquardt: 0.00001 New wR= 0.21430 Using Levenberg-Marquardt: 0.00010 New wR= 0.21428 Using Levenberg-Marquardt: 0.00100 New wR= 0.21409 Using Levenberg-Marquardt: 0.01000 New wR= 0.21300 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.33129 with corrections 0.18443 Rint for all data: 0.34556 with corrections 0.20041 0 observations identified as outliers and rejected Cycle 5 wR= 0.21300 Using Levenberg-Marquardt: 0.00100 New wR= 0.21503 Using Levenberg-Marquardt: 0.01000 New wR= 0.21374 Using Levenberg-Marquardt: 0.10000 New wR= 0.21222 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.33129 with corrections 0.18406 Rint for all data: 0.34556 with corrections 0.20005 0 observations identified as outliers and rejected Final wR= 0.21222 Final frame scales: Min= 0.8927 Max= 3.0838 Final absorption correction factors: Amin= 0.4919 Amax= 1.4784 PROFFIT INFO: Inet (after scale3 abspack): min=-1687.2250 max=1634445.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=48.7915 max=29676.4219 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/103 3317 reflections read from tmp file 850 reflections are rejected (786 as outliers, 64 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 79 61 51 45 28 26 22 27 77 Initial Chi^2= 2.30020 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.84689 Current error model SIG(F2)^2 = 486.69*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 412.17*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 412.17*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1634445- 115635 331 375153.09 32.18 100.00 114292- 4081 331 26981.00 6.95 84.29 4072- 2005 331 2690.15 2.69 29.91 2003- 1132 331 1521.77 1.99 15.41 1131- 744 331 905.91 1.34 1.21 744- 490 331 609.48 1.12 0.00 490- 294 331 386.94 1.03 0.91 294- 138 331 215.60 0.84 0.91 138- 12 331 70.03 0.46 0.00 11- -1687 338 -158.59 -0.34 0.00 ------------------------------------------------------------------------------------ 1634445- -1687 3317 40751.02 4.82 23.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 331 103883.39 11.10 52.87 1.59- 1.22 331 80855.96 8.60 41.09 1.22- 1.02 331 57721.29 6.31 30.51 1.02- 0.89 331 32402.78 3.91 17.22 0.89- 0.79 331 27042.30 3.55 13.60 0.79- 0.72 331 39406.99 4.46 23.56 0.72- 0.66 331 21218.99 2.99 12.08 0.66- 0.61 331 20077.09 2.88 15.11 0.61- 0.55 331 17393.96 2.65 16.92 0.55- 0.44 338 8195.97 1.77 9.47 ------------------------------------------------------------------------------------ 6.55- 0.44 3317 40751.02 4.82 23.21 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 331 103883.39 11.10 52.87 6.55- 1.22 662 92369.67 9.85 46.98 6.55- 1.02 993 80820.21 8.67 41.49 6.55- 0.89 1324 68715.85 7.48 35.42 6.55- 0.79 1655 60381.14 6.69 31.06 6.55- 0.72 1986 56885.45 6.32 29.81 6.55- 0.66 2317 51790.24 5.85 27.28 6.55- 0.61 2648 47826.10 5.48 25.76 6.55- 0.55 2979 44444.75 5.16 24.77 6.55- 0.44 3317 40751.02 4.82 23.21 ------------------------------------------------------------------------------------ 6.55- 0.44 3317 40751.02 4.82 23.21 Scale applied to data: s=0.611828 (maximum obs:1634445.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.200; Rsigma 0.049: data 3317 -> merged 485 With outlier rejection... Rint 0.179; Rsigma 0.050: data 3246 -> merged 485 Rejected total: 71, method kkm 67, method Blessing 4 Completeness direct cell (a, b, c) = (6.561, 6.561, 6.561), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445410, 6.561295 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.59 22 22 16.64 100.00 366 1.55 - 1.22 22 22 14.64 100.00 322 1.20 - 1.02 22 22 12.73 100.00 280 1.02 - 0.92 22 22 10.82 100.00 238 0.92 - 0.84 22 22 10.95 100.00 241 0.84 - 0.79 22 22 8.95 100.00 197 0.79 - 0.75 22 22 9.27 100.00 204 0.75 - 0.71 22 22 7.18 100.00 158 0.71 - 0.69 22 22 7.64 100.00 168 0.68 - 0.65 26 29 7.46 89.66 194 --------------------------------------------------------------- 7.36 - 0.65 224 227 10.57 98.68 2368 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:25:53 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.368699 7.361575 7.370705 120.1937 120.0322 89.7091 3246 Reflections read from file xs2212a.hkl 3246 Reflections used for space-group determination (up to diffraction limit of 0.47A); mean (I/sigma) = 4.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1632 1627 1623 1625 2441 2161 2165 3246 N (int>3sigma) = 0 177 187 252 176 308 494 503 731 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.9 22.7 24.7 23.7 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.5 4.9 4.7 Lattice type: P chosen Volume: 282.47 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.362 7.366 119.88 90.14 119.84 Niggli form: a.a = 53.943 b.b = 54.193 c.c = 54.260 b.c = -27.013 a.c = -0.131 a.b = -26.904 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.262 CUBIC F-lattice R(int) = 0.215 [ 3009] Vol = 1129.9 Cell: 10.389 10.442 10.415 90.05 89.83 90.06 Volume: 1129.87 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.254 RHOMBOHEDRAL R-lattice R(int) = 0.198 [ 2581] Vol = 847.4 Cell: 7.362 7.345 18.069 89.89 90.19 119.84 Volume: 847.40 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.254 RHOMBOHEDRAL R-lattice R(int) = 0.182 [ 826] Vol = 847.4 Trigonal Cell: 7.362 7.345 18.069 89.89 90.19 119.84 Volume: 847.40 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.399 TETRAGONAL I-lattice R(int) = 0.205 [ 2622] Vol = 564.9 Cell: 7.371 7.377 10.389 89.84 89.92 90.15 Volume: 564.94 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.446 TETRAGONAL I-lattice R(int) = 0.205 [ 2622] Vol = 564.9 Cell: 7.371 7.377 10.389 89.84 89.92 90.15 Volume: 564.94 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.429 ORTHORHOMBIC I-lattice R(int) = 0.159 [ 2551] Vol = 564.9 Cell: 7.371 10.389 7.377 89.84 89.85 90.08 Volume: 564.94 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.261 MONOCLINIC I-lattice R(int) = 0.155 [ 2045] Vol = 564.9 Cell: 10.389 7.371 7.377 90.15 90.16 90.08 Volume: 564.94 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.148 MONOCLINIC I-lattice R(int) = 0.152 [ 2029] Vol = 564.9 Cell: 7.366 7.345 10.442 90.00 90.08 89.86 Volume: 564.94 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.111 MONOCLINIC C-lattice R(int) = 0.179 [ 2060] Vol = 564.9 Cell: 10.389 10.442 7.345 90.00 134.85 90.06 Volume: 564.94 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) = 0.104 [ 1117] Vol = 282.5 Cell: 7.345 7.362 7.366 119.88 90.14 119.84 Volume: 282.47 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1623 0 2165 2154 3246 N (int>3sigma) = 0 0 0 0 252 0 503 502 731 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 24.7 24.5 23.7 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.9 4.7 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.848 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 242 617 N I>3s 0 0 0 151 0.1 0.1 -0.0 1.5 0.6 0.6 0.1 2.5 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 0.215 2795 Fd-3m 1 1 227 C N N N N 37 2284 0.215 2858 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.389403 10.442286 10.414651 90.0519 89.8321 90.0554 ZERR 1.00 0.005988 0.001005 0.010916 0.1048 0.0024 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 947284- 97422 358 339 48 7.1 347615.41 30.73 0.161 0.167 94206- 2625 436 420 48 8.8 13560.56 4.50 0.308 0.200 2608- 1553 495 491 48 10.2 2048.11 2.11 0.843 0.894 1528- 1030 523 512 48 10.7 1142.12 1.37 0.812 0.927 1018- 758 322 320 48 6.7 869.20 1.16 0.636 0.663 755- 568 326 320 48 6.7 628.74 0.98 0.651 0.731 567- 448 257 253 48 5.3 484.40 0.85 0.642 0.729 447- 308 242 236 48 4.9 351.29 0.71 0.714 0.858 306- 146 188 186 48 3.9 200.28 0.48 0.828 1.130 146- -318 170 169 53 3.2 55.89 0.21 0.958 2.671 ------------------------------------------------------------------------------------------- 947284- -318 3317 3246 485 6.7 38773.55 4.69 0.179 0.182 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-1.14 774 763 49 15.6 79702.68 8.89 0.174 0.186 0.027 1.13-0.89 585 563 50 11.3 41495.65 4.70 0.183 0.162 0.050 0.88-0.76 471 463 49 9.4 34755.30 4.21 0.197 0.216 0.066 0.76-0.69 378 370 48 7.7 27952.50 3.60 0.187 0.200 0.071 0.69-0.63 322 319 48 6.6 21152.56 2.97 0.175 0.190 0.090 0.63-0.59 259 252 48 5.3 10671.20 2.05 0.194 0.185 0.123 0.59-0.55 195 188 48 3.9 17510.73 2.68 0.172 0.181 0.104 0.55-0.52 137 135 48 2.8 5680.78 1.47 0.117 0.111 0.162 0.52-0.49 117 115 48 2.4 12701.41 2.38 0.079 0.081 0.114 0.49-0.45 79 78 49 1.6 3759.39 1.15 0.414 0.466 0.203 ------------------------------------------------------------------------------------------------------ inf-0.45 3317 3246 485 6.7 38773.55 4.69 0.179 0.182 0.050 inf-0.65 2419 2368 224 10.6 47885.10 5.56 0.180 0.186 0.043 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-1.14 763 49 49 100.0 15.6 79702.68 30.66 0.174 0.008 1.13-0.89 563 50 50 100.0 11.3 41495.65 13.91 0.183 0.022 0.88-0.76 463 49 49 100.0 9.4 34755.30 12.52 0.197 0.030 0.76-0.69 370 48 48 100.0 7.7 27952.50 10.07 0.187 0.030 0.69-0.63 319 51 48 94.1 6.6 21152.56 7.86 0.175 0.047 0.63-0.59 252 54 48 88.9 5.3 10671.20 4.61 0.194 0.058 0.59-0.55 188 55 48 87.3 3.9 17510.73 5.56 0.172 0.055 0.55-0.52 135 63 48 76.2 2.8 5680.78 2.41 0.117 0.089 0.52-0.49 115 79 48 60.8 2.4 12701.41 3.95 0.079 0.074 0.49-0.45 78 150 49 32.7 1.6 3759.39 1.46 0.414 0.855 -------------------------------------------------------------------------------------------- inf-0.45 3246 651 485 74.5 6.7 38773.55 14.28 0.179 0.027 inf-0.65 2368 227 224 98.7 10.6 47885.10 17.71 0.180 0.018 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.066409 0.012893 -0.008809 ( 0.000013 0.000014 0.000014 ) 0.014444 0.065227 -0.013231 ( 0.000012 0.000012 0.000013 ) 0.006093 -0.014659 -0.066250 ( 0.000015 0.000016 0.000016 ) M - matrix: 0.004656 -0.000003 -0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004636 -0.000005 ( 0.000001 0.000002 0.000001 ) -0.000010 -0.000005 0.004642 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.066409 0.012893 -0.008809 ( 0.000013 0.000014 0.000014 ) 0.014444 0.065227 -0.013231 ( 0.000012 0.000012 0.000013 ) 0.006093 -0.014659 -0.066250 ( 0.000015 0.000016 0.000016 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) unit cell: 10.3951(19) 10.418(2) 10.411(2) 89.933(17) 89.879(16) 89.958(16) V = 1127.4(4) unit cell: 10.4079(5) 10.4079(5) 10.4079(5) 90.0 90.0 90.0 V = 1127.44(10) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.150) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-557.0000 max=7904045.0000 PROFFIT INFO: signal sum lp corr: min=-576.8383 max=1106313.4880 PROFFIT INFO: background sum: min=62.0000 max=7519.0000 PROFFIT INFO: background sum sig2: min=450.0000 max=5482.0000 PROFFIT INFO: num of signal pixels: min=44 max=485 PROFFIT INFO: Inet: min=-922.9413 max=1770101.6250 PROFFIT INFO: sig(Inet): min=57.2785 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.70 max=197.69 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 612 2296 3450 4154 4446 5174 5592 5854 6294 6562 6634 Percent 9.2 34.6 52.0 62.6 67.0 78.0 84.3 88.2 94.9 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3317 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 3317 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1770102- 129139 331 403021.25 76.37 100.00 129039- 4014 331 30261.57 19.90 100.00 4008- 2099 331 2886.87 7.09 98.79 2096- 1231 331 1595.70 3.82 50.45 1229- 819 331 1001.58 2.28 12.39 819- 534 331 675.76 1.66 6.65 533- 326 331 427.43 1.24 5.14 325- 150 331 235.46 0.70 1.21 150- 13 331 76.59 0.29 0.00 13- -923 338 -136.95 -0.27 0.00 ------------------------------------------------------------------------------------ 1770102- -923 3317 43911.37 11.28 37.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 331 109366.46 14.60 66.77 1.73- 1.26 331 83404.54 21.85 59.82 1.26- 1.09 331 56131.00 17.58 63.14 1.09- 0.96 331 54000.13 14.75 35.35 0.96- 0.88 331 13394.51 6.21 41.09 0.88- 0.81 331 54953.45 15.24 38.37 0.81- 0.76 331 19214.49 5.95 18.13 0.76- 0.71 331 22191.57 7.18 18.43 0.71- 0.67 331 23774.29 7.90 27.79 0.67- 0.63 338 3537.10 1.77 5.62 ------------------------------------------------------------------------------------ 6.00- 0.63 3317 43911.37 11.28 37.38 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:25:53 2019 Sorting 3317 observations 43 unique observations with > 7.00 F2/sig(F2) 3317 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 24 332 Total number of frames 332 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3317 observations in 4 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 4 0 3 43 Total number of frames 43 789 observations > 7.00 F2/sig(F2) 789 observations in 4 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 4 0 2 42 Total number of frames 42 Removing 'redundancy=1' reflections Average redundancy: 15.7 (Out of 789 removed 3 = 786, unique = 50) 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 786 observations in 4 runs Run # start # end # total # 1 0 12 13 2 0 12 26 3 0 12 39 4 0 2 42 Total number of frames 42 50 unique data precomputed (should be 50) 50 unique data with 786 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 15.7 (Out of 786 removed 0 = 786, unique = 50) 50 unique data precomputed (should be 50) 50 unique data with 786 observations RMS deviation of equivalent data = 0.27004 Rint = 0.18921 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18275, wR= 0.24392 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08498, wR= 0.13769, Acormin=0.594, Acormax=1.343, Acor_av=0.994 F test: Probability=1.000, F= 4.593 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08208, wR= 0.13157, Acormin=0.543, Acormax=1.369, Acor_av=0.959 F test: Probability=0.811, F= 1.068 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08311, wR= 0.13253, Acormin=0.580, Acormax=1.403, Acor_av=0.966 F test: Probability=0.667, F= 1.033 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08140, wR= 0.12598, Acormin=0.509, Acormax=1.423, Acor_av=0.936 F test: Probability=0.824, F= 1.072 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07828, wR= 0.12105, Acormin=0.523, Acormax=1.432, Acor_av=0.934 F test: Probability=0.968, F= 1.148 Final absorption model (ne=4, no=3): Rint= 0.07828, Acormin=0.523, Acormax=1.432, Acor_av=0.934 Combined refinement in use Rint: 0.19138 There are 42 active scales (one needs to be fixed) Refinement control: frame scale #34 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 65 pars with 2145 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.27004 Using Levenberg-Marquardt: 0.00010 New wR= 0.12799 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18921 with corrections 0.08381 Rint for all data: 0.19138 with corrections 0.08664 4 observations identified as outliers and rejected Cycle 2 wR= 0.09560 Using Levenberg-Marquardt: 0.00001 New wR= 0.08221 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18209 with corrections 0.05659 Rint for all data: 0.19138 with corrections 0.06769 2 observations identified as outliers and rejected Cycle 3 wR= 0.07189 Using Levenberg-Marquardt: 0.00000 New wR= 0.07043 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18021 with corrections 0.05226 Rint for all data: 0.19138 with corrections 0.06630 0 observations identified as outliers and rejected Cycle 4 wR= 0.07043 Using Levenberg-Marquardt: 0.00000 New wR= 0.07065 Using Levenberg-Marquardt: 0.00000 New wR= 0.07065 Using Levenberg-Marquardt: 0.00001 New wR= 0.07065 Using Levenberg-Marquardt: 0.00010 New wR= 0.07065 Using Levenberg-Marquardt: 0.00100 New wR= 0.07065 Using Levenberg-Marquardt: 0.01000 New wR= 0.07065 Using Levenberg-Marquardt: 0.10000 New wR= 0.07066 Using Levenberg-Marquardt: 1.00000 New wR= 0.07057 Using Levenberg-Marquardt: 10.00000 New wR= 0.07045 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.18021 with corrections 0.05221 Rint for all data: 0.19138 with corrections 0.06627 Final wR= 0.07045 Final frame scales: Min= 0.8544 Max= 1.2780 Final absorption correction factors: Amin= 0.6030 Amax= 1.4209 PROFFIT INFO: Inet (after scale3 abspack): min=-927.6997 max=1350688.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=50.2303 max=24352.3691 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/103 3317 reflections read from tmp file 140 reflections are rejected (139 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 6 5 6 3 7 2 1 127 Initial Chi^2= 0.54689 Cycle 1, Chi^2= 1.02496 Current error model SIG(F2)^2 = 70.42*I_RAW + 9.78*I_BACK+(0.03920*)^2 Cycle 2, Chi^2= 1.02806 Current error model SIG(F2)^2 = 91.32*I_RAW + 5.73*I_BACK+(0.02888*)^2 Cycle 3, Chi^2= 1.01858 Current error model SIG(F2)^2 = 102.66*I_RAW + 4.06*I_BACK+(0.02492*)^2 Cycle 4, Chi^2= 1.00744 Current error model SIG(F2)^2 = 107.43*I_RAW + 3.53*I_BACK+(0.02391*)^2 Cycle 5, Chi^2= 1.00206 Current error model SIG(F2)^2 = 108.95*I_RAW + 3.40*I_BACK+(0.02372*)^2 Cycle 6, Chi^2= 1.00050 Current error model SIG(F2)^2 = 109.34*I_RAW + 3.37*I_BACK+(0.02368*)^2 Cycle 7, Chi^2= 1.00012 Current error model SIG(F2)^2 = 109.44*I_RAW + 3.36*I_BACK+(0.02367*)^2 Final Chi^2= 1.00012 Final error model SIG(F2)^2 = 109.44*I_RAW + 3.36*I_BACK+(0.02367*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1350688- 119872 331 387364.44 31.92 100.00 119112- 3620 331 30859.50 12.17 100.00 3617- 2048 331 2781.38 5.39 97.58 2046- 1184 331 1540.74 3.61 54.08 1182- 794 331 962.35 2.45 12.69 794- 526 331 661.89 2.13 7.55 526- 322 331 419.71 1.83 7.85 321- 148 331 231.77 1.36 2.11 148- 13 331 76.00 0.71 0.00 12- -928 338 -137.45 -0.57 0.00 ------------------------------------------------------------------------------------ 1350688- -928 3317 42386.10 6.08 38.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 331 106636.65 9.97 69.18 1.73- 1.26 331 80437.89 9.44 60.42 1.26- 1.09 331 55411.57 7.77 65.26 1.09- 0.96 331 51290.62 6.75 35.35 0.96- 0.88 331 13728.49 4.19 43.20 0.88- 0.81 331 52127.43 7.80 38.07 0.81- 0.76 331 18289.61 3.73 18.13 0.76- 0.71 331 20578.25 4.70 19.03 0.71- 0.67 331 22732.93 5.03 27.79 0.67- 0.63 338 3451.01 1.56 5.33 ------------------------------------------------------------------------------------ 6.00- 0.63 3317 42386.10 6.08 38.11 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 331 106636.65 9.97 69.18 6.00- 1.26 662 93537.27 9.71 64.80 6.00- 1.09 993 80828.70 9.06 64.95 6.00- 0.96 1324 73444.18 8.48 57.55 6.00- 0.88 1655 61501.04 7.63 54.68 6.00- 0.81 1986 59938.77 7.65 51.91 6.00- 0.76 2317 53988.89 7.09 47.09 6.00- 0.71 2648 49812.56 6.79 43.58 6.00- 0.67 2979 46803.72 6.60 41.83 6.00- 0.63 3317 42386.10 6.08 38.11 ------------------------------------------------------------------------------------ 6.00- 0.63 3317 42386.10 6.08 38.11 Scale applied to data: s=0.740362 (maximum obs:1350688.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.066; Rsigma 0.037: data 3317 -> merged 162 With outlier rejection... Rint 0.052; Rsigma 0.037: data 3301 -> merged 162 Rejected total: 16, method kkm 12, method Blessing 4 Completeness direct cell (a, b, c) = (10.408, 10.408, 10.408), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626483, 6.009016 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.76 14 14 21.57 100.00 302 1.73 - 1.27 14 14 24.07 100.00 337 1.26 - 1.06 14 14 26.64 100.00 373 1.05 - 0.97 14 14 23.36 100.00 327 0.95 - 0.88 14 14 24.43 100.00 342 0.87 - 0.81 14 14 21.36 100.00 299 0.80 - 0.76 14 14 22.93 100.00 321 0.76 - 0.72 14 14 19.00 100.00 266 0.72 - 0.69 14 14 20.71 100.00 290 0.69 - 0.65 19 19 17.63 100.00 335 --------------------------------------------------------------- 7.36 - 0.65 145 145 22.01 100.00 3192 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:25:53 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.368699 7.361575 7.370705 120.1937 120.0322 89.7091 3246 Reflections read from file xs2212a.hkl 3246 Reflections used for space-group determination (up to diffraction limit of 0.47A); mean (I/sigma) = 4.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1632 1627 1623 1625 2441 2161 2165 3246 N (int>3sigma) = 0 177 187 252 176 308 494 503 731 Mean intensity = 0.0 0.7 0.8 1.1 0.7 0.9 22.7 24.7 23.7 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.5 4.9 4.7 Lattice type: P chosen Volume: 282.47 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.362 7.366 119.88 90.14 119.84 Niggli form: a.a = 53.943 b.b = 54.193 c.c = 54.260 b.c = -27.013 a.c = -0.131 a.b = -26.904 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.262 CUBIC F-lattice R(int) = 0.215 [ 3009] Vol = 1129.9 Cell: 10.389 10.442 10.415 90.05 89.83 90.06 Volume: 1129.87 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.254 RHOMBOHEDRAL R-lattice R(int) = 0.198 [ 2581] Vol = 847.4 Cell: 7.362 7.345 18.069 89.89 90.19 119.84 Volume: 847.40 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.254 RHOMBOHEDRAL R-lattice R(int) = 0.182 [ 826] Vol = 847.4 Trigonal Cell: 7.362 7.345 18.069 89.89 90.19 119.84 Volume: 847.40 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.399 TETRAGONAL I-lattice R(int) = 0.205 [ 2622] Vol = 564.9 Cell: 7.371 7.377 10.389 89.84 89.92 90.15 Volume: 564.94 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.446 TETRAGONAL I-lattice R(int) = 0.205 [ 2622] Vol = 564.9 Cell: 7.371 7.377 10.389 89.84 89.92 90.15 Volume: 564.94 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.429 ORTHORHOMBIC I-lattice R(int) = 0.159 [ 2551] Vol = 564.9 Cell: 7.371 10.389 7.377 89.84 89.85 90.08 Volume: 564.94 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.261 MONOCLINIC I-lattice R(int) = 0.155 [ 2045] Vol = 564.9 Cell: 10.389 7.371 7.377 90.15 90.16 90.08 Volume: 564.94 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.148 MONOCLINIC I-lattice R(int) = 0.152 [ 2029] Vol = 564.9 Cell: 7.366 7.345 10.442 90.00 90.08 89.86 Volume: 564.94 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.111 MONOCLINIC C-lattice R(int) = 0.179 [ 2060] Vol = 564.9 Cell: 10.389 10.442 7.345 90.00 134.85 90.06 Volume: 564.94 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) = 0.104 [ 1117] Vol = 282.5 Cell: 7.345 7.362 7.366 119.88 90.14 119.84 Volume: 282.47 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1623 0 2165 2154 3246 N (int>3sigma) = 0 0 0 0 252 0 503 502 731 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 24.7 24.5 23.7 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.9 4.7 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.848 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 242 617 N I>3s 0 0 0 151 0.1 0.1 -0.0 1.5 0.6 0.6 0.1 2.5 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 0.215 2795 Fd-3m 1 1 227 C N N N N 37 2284 0.215 2858 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.389403 10.442286 10.414651 90.0519 89.8321 90.0554 ZERR 1.00 0.005988 0.001005 0.010916 0.1048 0.0024 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1153855- 94896 406 395 27 14.6 338978.81 29.75 0.047 0.057 74976- 1776 622 619 27 22.9 5499.84 7.52 0.104 0.146 1707- 768 650 649 27 24.0 1156.79 2.70 0.230 0.291 707- 359 597 596 27 22.1 523.46 1.85 0.384 0.540 358- 65 594 594 27 22.0 219.99 1.12 0.571 0.900 62- -165 448 448 27 16.6 -1.59 0.09 0.973 4.044 ------------------------------------------------------------------------------------------- 1153855- -165 3317 3301 162 20.4 41955.08 6.05 0.052 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-1.27 641 637 27 23.6 95542.92 9.94 0.049 0.056 0.027 1.26-0.97 704 700 28 25.0 49570.34 6.83 0.043 0.055 0.033 0.95-0.81 643 641 28 22.9 33935.10 6.15 0.049 0.055 0.043 0.80-0.73 573 570 27 21.1 17936.39 3.97 0.060 0.073 0.057 0.72-0.67 504 503 27 18.6 19619.11 4.40 0.086 0.109 0.066 0.66-0.63 252 250 25 10.0 4356.36 1.73 0.164 0.121 0.127 ------------------------------------------------------------------------------------------------------ inf-0.63 3317 3301 162 20.4 41955.08 6.05 0.052 0.062 0.037 inf-0.65 3204 3190 144 22.2 43163.92 6.19 0.051 0.059 0.037 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-1.27 637 27 27 100.0 23.6 95542.92 45.82 0.049 0.008 1.26-0.97 700 28 28 100.0 25.0 49570.34 31.92 0.043 0.008 0.95-0.81 641 28 28 100.0 22.9 33935.10 30.05 0.049 0.011 0.80-0.73 570 27 27 100.0 21.1 17936.39 16.57 0.060 0.015 0.72-0.67 503 27 27 100.0 18.6 19619.11 20.80 0.086 0.016 0.66-0.63 250 25 25 100.0 10.0 4356.36 5.79 0.164 0.044 -------------------------------------------------------------------------------------------- inf-0.63 3301 162 162 100.0 20.4 41955.08 27.91 0.052 0.011 inf-0.65 3190 144 144 100.0 22.2 43163.92 28.71 0.051 0.010 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:32:26 2019) ID: 3668; threads 40; handles 811; mem 514792.00 (1204688.00)kB; time: 1w 4d 23h 43m 14s MEMORY INFO: Memory PF:270.0, Ph:628.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.7,peak PF: 700.2, WS: 470.7, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:272.0, Ph:630.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.5,peak PF: 700.2, WS: 472.5, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:32:26 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000092 0.000065 0.000093 ) 0.064809 0.092374 0.027273 ( 0.000111 0.000078 0.000112 ) 0.045523 0.057900 0.132205 ( 0.000132 0.000093 0.000133 ) 7.38096 ( 0.00710 ) 7.36649 ( 0.00767 ) 7.42630 ( 0.00882 ) 120.52449 ( 0.11861 ) 120.40327 ( 0.11422 ) 89.27095 ( 0.08117 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:32:27 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000092 0.000065 0.000093 ) 0.064809 0.092374 0.027273 ( 0.000111 0.000078 0.000112 ) 0.045523 0.057900 0.132205 ( 0.000132 0.000093 0.000133 ) M - matrix: 0.013775 0.004545 0.009150 ( 0.000025 0.000016 0.000022 ) 0.004545 0.013992 0.009348 ( 0.000016 0.000019 0.000018 ) 0.009150 0.009348 0.018505 ( 0.000022 0.000018 0.000036 ) unit cell: 7.381(7) 7.366(8) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 22 | 0.943 ( 0.037) | 0.927 ( 0.094) | 1.330 ( 0.478) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 220 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.089 ( 0.813) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 204 obs out of 220 (total:220,skipped:0) (92.73%) UB - matrix: 0.087431 -0.046189 0.017571 ( 0.000091 0.000059 0.000090 ) 0.064802 0.092241 0.027387 ( 0.000081 0.000053 0.000080 ) 0.045554 0.057572 0.131874 ( 0.000106 0.000069 0.000104 ) M - matrix: 0.013919 0.004562 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004562 0.013956 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.371(6) 7.446(7) 120.46(9) 120.59(9) 89.14(7) V = 284.5(4) OTKP changes: 205 1 1 1 OTKP changes: 205 1 1 1 OTKP changes: 205 1 1 1 UB - matrix: 0.087499 -0.046089 0.017420 ( 0.000094 0.000061 0.000091 ) 0.064715 0.092382 0.027224 ( 0.000085 0.000055 0.000082 ) 0.045699 0.057898 0.132173 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013933 0.004592 0.009326 ( 0.000022 0.000013 0.000017 ) 0.004592 0.014011 0.009365 ( 0.000013 0.000014 0.000014 ) 0.009326 0.009365 0.018514 ( 0.000017 0.000014 0.000027 ) UB fit with 208 obs out of 220 (total:220,skipped:0) (94.55%) unit cell: 7.382(6) 7.366(6) 7.434(7) 120.53(9) 120.47(9) 89.22(7) V = 283.4(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1310 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087499 -0.046089 0.017420 ( 0.000094 0.000061 0.000091 ) 0.064715 0.092382 0.027224 ( 0.000085 0.000055 0.000082 ) 0.045699 0.057898 0.132173 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013933 0.004592 0.009326 ( 0.000022 0.000013 0.000017 ) 0.004592 0.014011 0.009365 ( 0.000013 0.000014 0.000014 ) 0.009326 0.009365 0.018514 ( 0.000017 0.000014 0.000027 ) UB fit with 208 obs out of 220 (total:220,skipped:0) (94.55%) unit cell: 7.382(6) 7.366(6) 7.434(7) 120.53(9) 120.47(9) 89.22(7) V = 283.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 214 obs out of 220 (total:220,skipped:0) (97.27%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.99 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.375) | 2.60- 1.75 | 21 | 0.822 ( 0.086) | 0.813 ( 0.150) | 0.732 ( 0.327) | 1.75- 1.57 | 21 | 0.859 ( 0.089) | 0.893 ( 0.144) | 0.679 ( 0.239) | 1.56- 1.35 | 21 | 0.953 ( 0.115) | 1.006 ( 0.139) | 1.063 ( 0.542) | 1.35- 1.16 | 21 | 0.962 ( 0.062) | 1.040 ( 0.102) | 0.917 ( 0.372) | 1.16- 1.00 | 21 | 0.937 ( 0.080) | 0.963 ( 0.179) | 0.959 ( 0.410) | 1.00- 0.88 | 21 | 0.969 ( 0.079) | 1.011 ( 0.129) | 1.194 ( 0.511) | 0.88- 0.79 | 21 | 0.979 ( 0.051) | 1.018 ( 0.136) | 1.175 ( 0.358) | 0.79- 0.69 | 21 | 0.980 ( 0.042) | 0.948 ( 0.110) | 1.240 ( 0.478) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.929 ( 0.097) | 1.357 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.941 ( 0.193) | 0.946 ( 0.157) | 1.098 ( 0.892) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.82 | 24 | 1.005 ( 0.047) | 1.008 ( 0.130) | 0.907 ( 0.354) | 0.79- 0.69 | 24 | 0.998 ( 0.044) | 1.006 ( 0.137) | 1.289 ( 0.497) | 0.69- 0.63 | 23 | 0.979 ( 0.051) | 0.913 ( 0.103) | 1.157 ( 0.432) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.510) | 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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb PROFFITPEAK info: 196 peaks in the peak location table UB fit with 17 obs out of 104 (total:104,skipped:0) (16.35%) UB - matrix: 0.085229 -0.045632 0.016843 ( 0.000743 0.000210 0.000361 ) 0.064106 0.092388 0.027180 ( 0.000950 0.000269 0.000462 ) 0.044641 0.057646 0.132040 ( 0.001911 0.000541 0.000929 ) M - matrix: 0.013366 0.004607 0.009072 ( 0.000245 0.000149 0.000261 ) 0.004607 0.013941 0.009354 ( 0.000149 0.000082 0.000101 ) 0.009072 0.009354 0.018457 ( 0.000261 0.000101 0.000247 ) unit cell: 7.52(5) 7.39(5) 7.41(7) 120.3(10) 120(1) 90.1(6) V = 290(4) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 4, #refl in peak table: 104 #indexed refl 97, indexation with best UB: 93.2692% Lattice: 7.4143 7.3608 7.3580 119.986 120.070 89.953 283.824 Rotation: -22.682 24.734 -35.058 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 101 obs out of 104 (total:104,skipped:0) (97.12%) UB - matrix: 0.087759 -0.044382 0.012618 ( 0.000150 0.000086 0.000085 ) 0.061603 0.094257 0.026143 ( 0.000153 0.000088 0.000086 ) 0.049265 0.055448 0.133199 ( 0.000128 0.000074 0.000073 ) M - matrix: 0.013924 0.004643 0.009280 ( 0.000035 0.000020 0.000020 ) 0.004643 0.013929 0.009290 ( 0.000020 0.000020 0.000014 ) 0.009280 0.009290 0.018585 ( 0.000020 0.000014 0.000020 ) unit cell: 7.359(10) 7.361(9) 7.355(6) 120.00(11) 119.96(11) 90.03(11) V = 281.8(6) OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 UB - matrix: 0.088022 -0.044245 0.012684 ( 0.000149 0.000088 0.000086 ) 0.061699 0.094357 0.026073 ( 0.000149 0.000088 0.000087 ) 0.049412 0.055476 0.133116 ( 0.000112 0.000066 0.000065 ) M - matrix: 0.013996 0.004668 0.009303 ( 0.000034 0.000020 0.000018 ) 0.004668 0.013939 0.009284 ( 0.000020 0.000020 0.000013 ) 0.009303 0.009284 0.018561 ( 0.000018 0.000013 0.000018 ) UB fit with 103 obs out of 104 (total:104,skipped:0) (99.04%) unit cell: 7.342(10) 7.357(9) 7.358(6) 119.95(10) 119.95(11) 90.09(10) V = 281.2(5) UB fit with 103 obs out of 104 (total:104,skipped:0) (99.04%) UB - matrix: 0.088022 -0.044245 0.012684 ( 0.000149 0.000088 0.000086 ) 0.061699 0.094357 0.026073 ( 0.000149 0.000088 0.000087 ) 0.049412 0.055476 0.133116 ( 0.000112 0.000066 0.000065 ) M - matrix: 0.013996 0.004668 0.009303 ( 0.000034 0.000020 0.000018 ) 0.004668 0.013939 0.009284 ( 0.000020 0.000020 0.000013 ) 0.009303 0.009284 0.018561 ( 0.000018 0.000013 0.000018 ) unit cell: 7.342(10) 7.357(9) 7.358(6) 119.95(10) 119.95(11) 90.09(10) V = 281.2(5) OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 UB - matrix: 0.088022 -0.044245 0.012684 ( 0.000149 0.000088 0.000086 ) 0.061699 0.094357 0.026073 ( 0.000149 0.000088 0.000087 ) 0.049412 0.055476 0.133116 ( 0.000112 0.000066 0.000065 ) M - matrix: 0.013996 0.004668 0.009303 ( 0.000034 0.000020 0.000018 ) 0.004668 0.013939 0.009284 ( 0.000020 0.000020 0.000013 ) 0.009303 0.009284 0.018561 ( 0.000018 0.000013 0.000018 ) UB fit with 103 obs out of 104 (total:104,skipped:0) (99.04%) unit cell: 7.342(10) 7.357(9) 7.358(6) 119.95(10) 119.95(11) 90.09(10) V = 281.2(5) 104 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Run 4 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.088022 -0.044245 0.012684 ( 0.000149 0.000088 0.000086 ) 0.061699 0.094357 0.026073 ( 0.000149 0.000088 0.000087 ) 0.049412 0.055476 0.133116 ( 0.000112 0.000066 0.000065 ) M - matrix: 0.013996 0.004668 0.009303 ( 0.000034 0.000020 0.000018 ) 0.004668 0.013939 0.009284 ( 0.000020 0.000020 0.000013 ) 0.009303 0.009284 0.018561 ( 0.000018 0.000013 0.000018 ) UB fit with 103 obs out of 104 (total:104,skipped:0) (99.04%) unit cell: 7.342(10) 7.357(9) 7.358(6) 119.95(10) 119.95(11) 90.09(10) V = 281.2(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 103 obs out of 104 (total:104,skipped:0) (99.04%) 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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb 0 of 99 peaks identified as outliers and rejected 99 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 99 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 99 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 2.60 | 10 | 0.862 ( 0.101) | 0.874 ( 0.133) | 1.045 ( 0.503) | 2.36- 1.75 | 10 | 0.875 ( 0.132) | 0.880 ( 0.170) | 0.831 ( 0.361) | 1.64- 1.49 | 10 | 0.936 ( 0.104) | 0.961 ( 0.150) | 0.905 ( 0.281) | 1.45- 1.35 | 10 | 0.920 ( 0.084) | 0.950 ( 0.129) | 0.665 ( 0.216) | 1.35- 1.14 | 10 | 0.939 ( 0.079) | 0.933 ( 0.092) | 0.795 ( 0.359) | 1.14- 1.00 | 10 | 0.949 ( 0.091) | 0.982 ( 0.100) | 0.985 ( 0.336) | 1.00- 0.87 | 10 | 0.998 ( 0.047) | 1.000 ( 0.065) | 0.929 ( 0.287) | 0.86- 0.78 | 10 | 0.994 ( 0.040) | 1.009 ( 0.096) | 1.256 ( 0.397) | 0.75- 0.69 | 10 | 0.971 ( 0.050) | 0.950 ( 0.084) | 1.187 ( 0.421) | 0.69- 0.63 | 9 | 0.953 ( 0.042) | 0.888 ( 0.043) | 1.320 ( 0.466) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 0.63 | 99 | 0.939 ( 0.093) | 0.943 ( 0.122) | 0.988 ( 0.421) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) UB - matrix: 0.088043 -0.044191 0.012955 ( 0.000083 0.000052 0.000050 ) 0.061489 0.094500 0.025999 ( 0.000070 0.000043 0.000042 ) 0.049307 0.055427 0.133122 ( 0.000048 0.000030 0.000029 ) M - matrix: 0.013964 0.004653 0.009303 ( 0.000018 0.000010 0.000009 ) 0.004653 0.013955 0.009263 ( 0.000010 0.000010 0.000006 ) 0.009303 0.009263 0.018565 ( 0.000009 0.000006 0.000008 ) unit cell: 7.354(5) 7.342(5) 7.353(3) 119.84(5) 120.04(5) 90.07(5) V = 281.1(3) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: 0.087855 -0.044334 0.012719 ( 0.000069 0.000043 0.000042 ) 0.061581 0.094398 0.026169 ( 0.000054 0.000033 0.000032 ) 0.049346 0.055464 0.133209 ( 0.000046 0.000029 0.000028 ) M - matrix: 0.013946 0.004655 0.009302 ( 0.000015 0.000008 0.000008 ) 0.004655 0.013953 0.009295 ( 0.000008 0.000008 0.000006 ) 0.009302 0.009295 0.018591 ( 0.000008 0.000006 0.000008 ) UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) unit cell: 7.359(4) 7.353(4) 7.357(2) 119.96(4) 120.02(5) 90.03(4) V = 281.5(2) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 99 obs out of 99 (total:99,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb 0 of 98 peaks identified as outliers and rejected 98 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 98 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 98 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 2.59 | 10 | 0.846 ( 0.104) | 0.859 ( 0.130) | 1.048 ( 0.500) | 2.38- 1.75 | 10 | 0.877 ( 0.134) | 0.881 ( 0.172) | 0.823 ( 0.374) | 1.75- 1.56 | 10 | 0.924 ( 0.098) | 0.952 ( 0.149) | 0.904 ( 0.284) | 1.50- 1.35 | 10 | 0.964 ( 0.064) | 0.995 ( 0.097) | 0.633 ( 0.249) | 1.35- 1.14 | 10 | 0.923 ( 0.091) | 0.926 ( 0.112) | 0.794 ( 0.355) | 1.14- 1.00 | 10 | 0.947 ( 0.100) | 0.985 ( 0.098) | 0.974 ( 0.323) | 1.00- 0.87 | 10 | 0.999 ( 0.047) | 1.007 ( 0.070) | 0.956 ( 0.350) | 0.87- 0.75 | 10 | 0.990 ( 0.041) | 1.006 ( 0.097) | 1.240 ( 0.386) | 0.73- 0.69 | 10 | 0.967 ( 0.055) | 0.949 ( 0.097) | 1.244 ( 0.488) | 0.68- 0.63 | 8 | 0.959 ( 0.042) | 0.906 ( 0.062) | 1.222 ( 0.421) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 0.63 | 98 | 0.939 ( 0.096) | 0.947 ( 0.124) | 0.979 ( 0.428) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.1 | 80 | 0.979 ( 0.036) | 1.027 ( 0.072) | 1.125 ( 0.506) | 10.3-14.9 | 80 | 0.981 ( 0.043) | 1.040 ( 0.071) | 1.206 ( 0.570) | 14.9-18.8 | 80 | 0.995 ( 0.235) | 1.021 ( 0.101) | 1.221 ( 1.202) | 18.9-23.5 | 80 | 0.955 ( 0.057) | 1.000 ( 0.084) | 0.931 ( 0.423) | 23.5-27.1 | 80 | 0.961 ( 0.061) | 0.994 ( 0.093) | 0.948 ( 0.418) | 27.2-32.2 | 80 | 0.941 ( 0.091) | 0.949 ( 0.112) | 0.942 ( 0.482) | 32.4-36.3 | 80 | 0.928 ( 0.169) | 0.916 ( 0.133) | 1.076 ( 0.669) | 36.3-38.6 | 80 | 0.876 ( 0.095) | 0.839 ( 0.124) | 1.028 ( 0.497) | 38.7-41.9 | 80 | 0.892 ( 0.093) | 0.851 ( 0.131) | 1.030 ( 0.475) | 42.0-50.1 | 83 | 0.876 ( 0.118) | 0.802 ( 0.135) | 0.969 ( 0.485) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 803 | 0.938 ( 0.123) | 0.943 ( 0.136) | 1.047 ( 0.622) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.13 e2 dimension: a=-0.0070 b=1.24 e3 dimension: a=0.0005 b=1.09 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3814 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:32:39 2019 PROFFITMAIN - Started at Wed Aug 21 13:32:39 2019 OTKP changes: 320 2 3 4 OTKP changes: 320 2 3 4 OTKP changes: 320 2 3 4 UB - matrix: 0.087577 -0.046026 0.016800 ( 0.000086 0.000064 0.000088 ) 0.063363 0.092456 0.026867 ( 0.000101 0.000075 0.000103 ) 0.045256 0.057651 0.131994 ( 0.000104 0.000077 0.000106 ) M - matrix: 0.013733 0.004436 0.009147 ( 0.000022 0.000014 0.000018 ) 0.004436 0.013990 0.009320 ( 0.000014 0.000017 0.000016 ) 0.009147 0.009320 0.018427 ( 0.000018 0.000016 0.000029 ) UB fit with 368 obs out of 803 (total:803,skipped:0) (45.83%) unit cell: 7.400(7) 7.366(7) 7.433(7) 120.76(10) 120.30(10) 88.82(7) V = 284.8(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) UB - matrix: 0.087567 -0.046175 0.017314 ( 0.000101 0.000063 0.000096 ) 0.064568 0.092359 0.027155 ( 0.000089 0.000055 0.000084 ) 0.045799 0.057750 0.132076 ( 0.000107 0.000066 0.000102 ) M - matrix: 0.013934 0.004565 0.009318 ( 0.000023 0.000013 0.000018 ) 0.004565 0.013997 0.009336 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009336 0.018481 ( 0.000018 0.000014 0.000028 ) unit cell: 7.381(7) 7.363(6) 7.439(7) 120.51(9) 120.53(10) 89.12(7) V = 283.5(4) OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 UB - matrix: 0.087287 -0.045968 0.017391 ( 0.000097 0.000061 0.000091 ) 0.064681 0.092329 0.027289 ( 0.000085 0.000053 0.000080 ) 0.045556 0.057802 0.132015 ( 0.000105 0.000065 0.000099 ) M - matrix: 0.013878 0.004593 0.009297 ( 0.000022 0.000013 0.000018 ) 0.004593 0.013979 0.009351 ( 0.000013 0.000014 0.000014 ) 0.009297 0.009351 0.018475 ( 0.000018 0.000014 0.000027 ) UB fit with 201 obs out of 212 (total:212,skipped:0) (94.81%) unit cell: 7.396(6) 7.377(6) 7.441(7) 120.53(9) 120.42(9) 89.30(7) V = 284.7(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.170) HKL list info: 1290 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087287 -0.045968 0.017392 ( 0.000097 0.000061 0.000091 ) 0.064681 0.092329 0.027289 ( 0.000085 0.000053 0.000080 ) 0.045556 0.057802 0.132015 ( 0.000105 0.000065 0.000099 ) M - matrix: 0.013878 0.004593 0.009297 ( 0.000022 0.000013 0.000018 ) 0.004593 0.013979 0.009351 ( 0.000013 0.000014 0.000014 ) 0.009297 0.009351 0.018475 ( 0.000018 0.000014 0.000027 ) UB fit with 201 obs out of 212 (total:212,skipped:0) (94.81%) unit cell: 7.396(6) 7.377(6) 7.441(7) 120.53(9) 120.42(9) 89.30(7) V = 284.7(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 206 obs out of 212 (total:212,skipped:0) (97.17%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.117957 0.039147 0.078729 ( 0.000074 0.000046 0.000069 ) 0.000019 0.111496 0.056205 ( 0.000076 0.000048 0.000071 ) -0.000015 -0.000042 0.095425 ( 0.000088 0.000055 0.000082 ) M - matrix: 0.013914 0.004620 0.009286 ( 0.000017 0.000010 0.000014 ) 0.004620 0.013964 0.009345 ( 0.000010 0.000011 0.000011 ) 0.009286 0.009345 0.018463 ( 0.000014 0.000011 0.000021 ) UB fit with 206 obs out of 212 (total:212,skipped:0) (97.17%) unit cell: 7.378(5) 7.381(5) 7.431(8) 120.47(9) 120.25(9) 89.50(5) V = 284.3(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.087804 -0.044309 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094149 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055798 0.133161 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004658 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009312 0.018585 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3551(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1268 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) UB - matrix: 0.087873 -0.044330 0.012734 ( 0.000073 0.000045 0.000043 ) 0.061592 0.094410 0.026173 ( 0.000057 0.000034 0.000033 ) 0.049346 0.055447 0.133196 ( 0.000044 0.000027 0.000026 ) M - matrix: 0.013950 0.004656 0.009304 ( 0.000015 0.000008 0.000008 ) 0.004656 0.013953 0.009292 ( 0.000008 0.000008 0.000005 ) 0.009304 0.009292 0.018588 ( 0.000008 0.000005 0.000007 ) unit cell: 7.358(4) 7.352(4) 7.357(2) 119.95(4) 120.02(5) 90.03(5) V = 281.4(2) 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 4 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 717 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: 0.087873 -0.044330 0.012734 ( 0.000073 0.000045 0.000043 ) 0.061592 0.094410 0.026173 ( 0.000057 0.000034 0.000033 ) 0.049346 0.055447 0.133196 ( 0.000044 0.000027 0.000026 ) M - matrix: 0.013950 0.004656 0.009304 ( 0.000015 0.000008 0.000008 ) 0.004656 0.013953 0.009292 ( 0.000008 0.000008 0.000005 ) 0.009304 0.009292 0.018588 ( 0.000008 0.000005 0.000007 ) UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) unit cell: 7.358(4) 7.352(4) 7.357(2) 119.95(4) 120.02(5) 90.03(5) V = 281.4(2) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 68.89 ph= 0.28 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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117740 0.038899 0.078593 ( 0.000040 0.000037 0.000044 ) 0.000024 0.111473 0.056083 ( 0.000028 0.000026 0.000031 ) -0.000068 -0.000124 0.096148 ( 0.000031 0.000029 0.000034 ) M - matrix: 0.013863 0.004583 0.009248 ( 0.000009 0.000006 0.000007 ) 0.004583 0.013939 0.009297 ( 0.000006 0.000007 0.000006 ) 0.009248 0.009297 0.018567 ( 0.000007 0.000006 0.000010 ) UB fit with 796 obs out of 803 (total:803,skipped:0) (99.13%) unit cell: 7.373(3) 7.362(2) 7.370(3) 120.18(4) 120.06(4) 89.70(3) V = 282.52(17) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 84 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof 3570 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:32:45 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.170) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-534.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-608.7542 max=1110007.4327 PROFFIT INFO: background sum: min=-47.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=432.0000 max=5606.0000 PROFFIT INFO: num of signal pixels: min=43 max=496 PROFFIT INFO: Inet: min=-974.0068 max=1776011.8750 PROFFIT INFO: sig(Inet): min=57.5968 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.66 max=198.21 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 301 1222 1864 2232 2397 2788 3013 3147 3385 3529 3570 Percent 8.4 34.2 52.2 62.5 67.1 78.1 84.4 88.2 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3570 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 3570 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1776012- 131759 357 398315.67 77.35 100.00 131670- 3928 357 31300.84 19.87 100.00 3920- 2044 357 2834.19 6.94 98.32 2044- 1210 357 1568.88 3.78 50.98 1210- 815 357 989.99 2.24 12.32 814- 554 357 674.59 1.64 6.44 552- 327 357 431.92 1.25 5.32 326- 152 357 236.32 0.71 1.40 152- 20 357 81.65 0.30 0.00 19- -974 357 -133.50 -0.26 0.00 ------------------------------------------------------------------------------------ 1776012- -974 3570 43630.06 11.38 37.48 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 357 102248.36 17.89 69.47 1.59- 1.22 357 84414.22 19.79 56.86 1.22- 1.02 357 57547.33 16.37 50.98 1.02- 0.89 357 34940.09 10.64 38.10 0.89- 0.80 357 27307.21 8.74 30.25 0.80- 0.73 357 45378.09 13.32 42.02 0.73- 0.66 357 25332.99 8.02 26.33 0.66- 0.61 357 23916.55 7.36 24.65 0.61- 0.55 357 22809.43 7.39 21.85 0.55- 0.44 357 12406.29 4.32 14.29 ------------------------------------------------------------------------------------ 6.55- 0.44 3570 43630.06 11.38 37.48 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:32:45 2019 Sorting 3570 observations 87 unique observations with > 7.00 F2/sig(F2) 3570 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 49 357 Total number of frames 357 Maximum number of 87 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 3570 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 9 73 Total number of frames 73 850 observations > 7.00 F2/sig(F2) 850 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 9 73 Total number of frames 73 Removing 'redundancy=1' reflections Average redundancy: 6.7 (Out of 850 removed 35 = 815, unique = 122) 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 815 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 9 73 Total number of frames 73 122 unique data precomputed (should be 122) 122 unique data with 815 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.7 (Out of 815 removed 0 = 815, unique = 122) 122 unique data precomputed (should be 122) 122 unique data with 815 observations RMS deviation of equivalent data = 0.37068 Rint = 0.33306 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.33238, wR= 0.45419 Trying model 1 (ne=2, no=0)... Results: Rint= 0.25273, wR= 0.34163, Acormin=0.562, Acormax=1.459, Acor_av=1.003 F test: Probability=1.000, F= 1.717 Trying model 2 (ne=2, no=1)... Results: Rint= 0.24983, wR= 0.34119, Acormin=0.536, Acormax=1.480, Acor_av=0.949 F test: Probability=0.597, F= 1.019 Trying model 3 (ne=4, no=0)... Results: Rint= 0.25012, wR= 0.33952, Acormin=0.536, Acormax=1.505, Acor_av=0.966 F test: Probability=0.539, F= 1.008 Trying model 4 (ne=4, no=1)... Results: Rint= 0.24362, wR= 0.33711, Acormin=0.408, Acormax=1.399, Acor_av=0.925 F test: Probability=0.766, F= 1.057 Trying model 5 (ne=4, no=3)... Results: Rint= 0.23970, wR= 0.31503, Acormin=0.293, Acormax=1.611, Acor_av=0.837 F test: Probability=0.844, F= 1.081 Trying model 6 (ne=6, no=0)... Results: Rint= 0.25107, wR= 0.32077, Acormin=0.253, Acormax=1.535, Acor_av=0.911 F test: Probability=0.000, F= 0.981 Trying model 7 (ne=6, no=1)... Results: Rint= 0.24144, wR= 0.31220, Acormin=0.215, Acormax=1.565, Acor_av=0.902 F test: Probability=0.760, F= 1.056 Trying model 8 (ne=6, no=3)... Results: Rint= 0.24020, wR= 0.29972, Acormin=0.101, Acormax=1.745, Acor_av=0.809 F test: Probability=0.757, F= 1.055 Trying model 9 (ne=6, no=5)... Results: Rint= 0.24327, wR= 0.30893, Acormin=0.192, Acormax=2.261, Acor_av=0.691 F test: Probability=0.560, F= 1.012 Trying model 10 (ne=8, no=0)... Results: Rint= 0.25129, wR= 0.31152, Acormin=0.094, Acormax=1.614, Acor_av=0.859 F test: Probability=0.000, F= 0.954 Trying model 11 (ne=8, no=1)... Results: Rint= 0.29622, wR= 0.36264, Acormin=-0.025, Acormax=1.289, Acor_av=0.606 F test: Probability=0.000, F= 0.683 Trying model 12 (ne=8, no=3)... Results: Rint= 0.29234, wR= 0.34613, Acormin=0.001, Acormax=0.111, Acor_av=0.045 F test: Probability=0.000, F= 0.694 Trying model 13 (ne=8, no=5)... Results: Rint= 0.26307, wR= 0.32152, Acormin=0.001, Acormax=0.110, Acor_av=0.048 F test: Probability=0.000, F= 0.842 Trying model 14 (ne=8, no=7)... Results: Rint= 0.21527, wR= 0.28072, Acormin=-0.013, Acormax=0.123, Acor_av=0.051 F test: Probability=0.995, F= 1.228 Final absorption model (ne=2, no=0): Rint= 0.25273, Acormin=0.562, Acormax=1.459, Acor_av=1.003 Combined refinement in use Rint: 0.34708 There are 73 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 77 pars with 3003 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.37068 Using Levenberg-Marquardt: 0.00010 New wR= 0.22567 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33306 with corrections 0.19327 Rint for all data: 0.34708 with corrections 0.20882 1 observations identified as outliers and rejected Cycle 2 wR= 0.22084 Using Levenberg-Marquardt: 0.00001 New wR= 0.20762 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33284 with corrections 0.18072 Rint for all data: 0.34708 with corrections 0.19872 0 observations identified as outliers and rejected Cycle 3 wR= 0.20762 Using Levenberg-Marquardt: 0.00000 New wR= 0.20368 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33284 with corrections 0.17864 Rint for all data: 0.34708 with corrections 0.19686 0 observations identified as outliers and rejected Cycle 4 wR= 0.20368 Using Levenberg-Marquardt: 0.00000 New wR= 0.20340 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33284 with corrections 0.17813 Rint for all data: 0.34708 with corrections 0.19644 0 observations identified as outliers and rejected Cycle 5 wR= 0.20340 Using Levenberg-Marquardt: 0.00000 New wR= 0.20355 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.33284 with corrections 0.17820 Rint for all data: 0.34708 with corrections 0.19658 Final wR= 0.20355 Final frame scales: Min= 0.7405 Max= 2.7414 Final absorption correction factors: Amin= 0.6231 Amax= 1.3950 PROFFIT INFO: Inet (after scale3 abspack): min=-1494.2335 max=1387000.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=50.4453 max=25490.0293 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/103 3570 reflections read from tmp file 903 reflections are rejected (845 as outliers, 58 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 81 62 35 42 34 31 18 16 103 Initial Chi^2= 2.26689 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88676 Current error model SIG(F2)^2 = 469.49*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 416.33*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 416.33*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1387000- 119776 357 372818.70 32.13 100.00 119674- 3877 357 27579.72 6.84 83.75 3875- 1967 357 2641.91 2.69 29.13 1961- 1144 357 1506.95 1.93 14.29 1144- 748 357 921.77 1.33 1.12 747- 499 357 618.57 1.12 0.28 498- 297 357 390.92 1.01 0.56 297- 142 357 219.86 0.84 0.56 141- 18 357 75.72 0.50 0.28 17- -1494 357 -145.06 -0.32 0.00 ------------------------------------------------------------------------------------ 1387000- -1494 3570 40662.91 4.81 23.00 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 357 105401.43 11.27 52.10 1.59- 1.22 357 80657.79 8.61 40.06 1.22- 1.02 357 55892.46 6.28 31.65 1.02- 0.89 357 32700.50 3.87 16.53 0.89- 0.80 357 24605.96 3.24 12.61 0.80- 0.73 357 40570.16 4.63 23.53 0.73- 0.66 357 21273.81 2.97 13.17 0.66- 0.61 357 19488.05 2.76 13.73 0.61- 0.55 357 17993.16 2.72 17.37 0.55- 0.44 357 8045.74 1.74 9.24 ------------------------------------------------------------------------------------ 6.55- 0.44 3570 40662.91 4.81 23.00 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.59 357 105401.43 11.27 52.10 6.55- 1.22 714 93029.61 9.94 46.08 6.55- 1.02 1071 80650.56 8.72 41.27 6.55- 0.89 1428 68663.05 7.51 35.08 6.55- 0.80 1785 59851.63 6.65 30.59 6.55- 0.73 2142 56638.05 6.32 29.41 6.55- 0.66 2499 51586.02 5.84 27.09 6.55- 0.61 2856 47573.77 5.45 25.42 6.55- 0.55 3213 44287.04 5.15 24.53 6.55- 0.44 3570 40662.91 4.81 23.00 ------------------------------------------------------------------------------------ 6.55- 0.44 3570 40662.91 4.81 23.00 Scale applied to data: s=0.720980 (maximum obs:1387000.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.197; Rsigma 0.049: data 3570 -> merged 485 With outlier rejection... Rint 0.188; Rsigma 0.050: data 3518 -> merged 485 Rejected total: 52, method kkm 48, method Blessing 4 Completeness direct cell (a, b, c) = (6.562, 6.562, 6.562), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445438, 6.561716 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.59 22 22 18.00 100.00 396 1.55 - 1.22 22 22 16.14 100.00 355 1.20 - 1.02 22 22 13.91 100.00 306 1.02 - 0.92 22 22 11.91 100.00 262 0.92 - 0.84 22 22 12.23 100.00 269 0.84 - 0.79 22 22 9.45 100.00 208 0.79 - 0.75 22 22 10.00 100.00 220 0.75 - 0.71 22 22 7.86 100.00 173 0.71 - 0.69 22 22 8.18 100.00 180 0.68 - 0.65 26 29 8.00 89.66 208 --------------------------------------------------------------- 7.36 - 0.65 224 227 11.50 98.68 2577 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:32:46 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.372669 7.361574 7.369788 120.1840 120.0611 89.7013 3518 Reflections read from file xs2212a.hkl 3518 Reflections used for space-group determination (up to diffraction limit of 0.47A); mean (I/sigma) = 4.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1768 1763 1765 1756 2648 2337 2346 3518 N (int>3sigma) = 0 199 203 278 192 340 534 548 795 Mean intensity = 0.0 0.9 0.9 1.3 0.9 1.0 26.9 28.9 28.0 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.5 4.9 4.7 Lattice type: P chosen Volume: 282.52 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.362 7.364 119.86 90.11 119.85 Niggli form: a.a = 53.952 b.b = 54.193 c.c = 54.235 b.c = -26.994 a.c = -0.102 a.b = -26.915 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.244 CUBIC F-lattice R(int) = 0.216 [ 3280] Vol = 1130.1 Cell: 10.391 10.446 10.411 90.07 89.85 90.09 Volume: 1130.09 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.240 RHOMBOHEDRAL R-lattice R(int) = 0.199 [ 2852] Vol = 847.6 Cell: 7.362 7.345 18.073 89.92 90.21 119.85 Volume: 847.57 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.240 RHOMBOHEDRAL R-lattice R(int) = 0.188 [ 919] Vol = 847.6 Trigonal Cell: 7.362 7.345 18.073 89.92 90.21 119.85 Volume: 847.57 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.464 TETRAGONAL I-lattice R(int) = 0.203 [ 2892] Vol = 565.0 Cell: 7.370 7.378 10.391 89.83 89.96 90.19 Volume: 565.04 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.488 TETRAGONAL I-lattice R(int) = 0.203 [ 2892] Vol = 565.0 Cell: 7.370 7.378 10.391 89.83 89.96 90.19 Volume: 565.04 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.400 ORTHORHOMBIC I-lattice R(int) = 0.171 [ 2822] Vol = 565.0 Cell: 7.370 10.391 7.378 89.83 89.81 90.04 Volume: 565.04 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.248 MONOCLINIC I-lattice R(int) = 0.169 [ 2311] Vol = 565.0 Cell: 10.391 7.370 7.378 90.19 90.17 90.04 Volume: 565.04 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.118 MONOCLINIC I-lattice R(int) = 0.159 [ 2298] Vol = 565.0 Cell: 7.364 7.345 10.446 89.99 90.11 89.89 Volume: 565.04 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.170 MONOCLINIC C-lattice R(int) = 0.165 [ 2321] Vol = 565.0 Cell: 10.391 10.446 7.345 89.99 134.87 90.09 Volume: 565.04 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) = 0.123 [ 1368] Vol = 282.5 Cell: 7.345 7.362 7.364 119.86 90.11 119.85 Volume: 282.52 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1765 0 2346 2333 3518 N (int>3sigma) = 0 0 0 0 278 0 548 543 795 Mean intensity = 0.0 0.0 0.0 0.0 1.3 0.0 28.9 29.1 28.0 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.9 4.8 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.975 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 21 21 262 674 N I>3s 0 0 0 164 0.0 0.0 -0.0 1.8 0.6 0.6 0.1 2.5 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 0.215 3046 Fd-3m 1 1 227 C N N N N 37 2284 0.217 3110 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.391493 10.445808 10.411046 90.0658 89.8502 90.0863 ZERR 1.00 0.005954 0.001006 0.010808 0.1014 0.0026 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 888121- 102316 393 370 48 7.7 346418.16 30.54 0.170 0.179 101624- 2608 446 442 48 9.2 13392.14 4.33 0.315 0.195 2606- 1441 574 569 48 11.9 2062.90 2.20 0.843 0.927 1417- 1023 575 571 48 11.9 1140.39 1.40 0.822 0.933 1018- 745 341 340 48 7.1 859.49 1.16 0.606 0.647 738- 611 322 316 48 6.6 623.58 0.92 0.622 0.676 610- 464 294 291 48 6.1 522.45 0.83 0.686 0.810 461- 320 249 245 48 5.1 382.54 0.74 0.703 0.794 318- 152 220 219 48 4.6 215.57 0.50 0.806 1.118 148- -300 156 155 53 2.9 47.55 0.18 0.967 2.823 ------------------------------------------------------------------------------------------- 888121- -300 3570 3518 485 7.3 38859.75 4.69 0.188 0.192 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-1.14 825 815 48 17.0 81742.15 9.06 0.198 0.215 0.026 1.14-0.89 648 638 51 12.5 39071.92 4.60 0.189 0.189 0.052 0.88-0.76 506 499 49 10.2 34932.45 4.15 0.175 0.184 0.066 0.76-0.69 407 402 48 8.4 28608.34 3.63 0.171 0.191 0.073 0.69-0.63 361 357 50 7.1 19238.14 2.77 0.191 0.185 0.092 0.63-0.58 290 284 51 5.6 11049.31 2.01 0.233 0.244 0.122 0.58-0.54 204 198 49 4.0 18812.29 2.82 0.134 0.131 0.103 0.54-0.52 139 137 48 2.9 3842.07 1.21 0.139 0.146 0.213 0.52-0.49 121 120 49 2.4 14049.33 2.45 0.082 0.092 0.114 0.49-0.45 69 68 42 1.6 4204.35 1.18 0.422 0.494 0.197 ------------------------------------------------------------------------------------------------------ inf-0.45 3570 3518 485 7.3 38859.75 4.69 0.188 0.192 0.050 inf-0.65 2612 2577 224 11.5 47775.22 5.55 0.191 0.202 0.043 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-1.14 815 48 48 100.0 17.0 81742.15 34.07 0.198 0.009 1.14-0.89 638 51 51 100.0 12.5 39071.92 14.52 0.189 0.021 0.88-0.76 499 49 49 100.0 10.2 34932.45 12.77 0.175 0.029 0.76-0.69 402 48 48 100.0 8.4 28608.34 10.48 0.171 0.029 0.69-0.63 357 53 50 94.3 7.1 19238.14 7.62 0.191 0.045 0.63-0.58 284 58 51 87.9 5.6 11049.31 4.62 0.233 0.055 0.58-0.54 198 56 49 87.5 4.0 18812.29 5.91 0.134 0.053 0.54-0.52 137 65 48 73.8 2.9 3842.07 2.10 0.139 0.119 0.52-0.49 120 82 49 59.8 2.4 14049.33 4.10 0.082 0.072 0.49-0.45 68 138 42 30.4 1.6 4204.35 1.47 0.422 0.923 -------------------------------------------------------------------------------------------- inf-0.45 3518 649 485 74.7 7.3 38859.75 15.26 0.188 0.027 inf-0.65 2577 227 224 98.7 11.5 47775.22 18.93 0.191 0.018 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.066376 0.012931 -0.008883 ( 0.000012 0.000013 0.000013 ) 0.014500 0.065225 -0.013196 ( 0.000011 0.000012 0.000012 ) 0.006128 -0.014649 -0.066265 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004654 -0.000002 -0.000008 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004636 -0.000005 ( 0.000001 0.000002 0.000001 ) -0.000008 -0.000005 0.004644 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.066376 0.012931 -0.008883 ( 0.000012 0.000013 0.000013 ) 0.014500 0.065225 -0.013196 ( 0.000011 0.000012 0.000012 ) 0.006128 -0.014649 -0.066265 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) unit cell: 10.3977(18) 10.417(2) 10.408(2) 89.940(16) 89.904(15) 89.971(15) V = 1127.4(4) unit cell: 10.4077(5) 10.4077(5) 10.4077(5) 90.0 90.0 90.0 V = 1127.36(9) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.170) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-534.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-608.7542 max=1110007.4327 PROFFIT INFO: background sum: min=-47.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=432.0000 max=5606.0000 PROFFIT INFO: num of signal pixels: min=43 max=496 PROFFIT INFO: Inet: min=-974.0068 max=1776011.8750 PROFFIT INFO: sig(Inet): min=57.5968 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.66 max=198.21 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 602 2444 3728 4464 4794 5576 6026 6294 6770 7058 7140 Percent 8.4 34.2 52.2 62.5 67.1 78.1 84.4 88.2 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3570 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 3570 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1776012- 131759 357 398315.67 77.35 100.00 131670- 3928 357 31300.84 19.87 100.00 3920- 2044 357 2834.19 6.94 98.32 2044- 1210 357 1568.88 3.78 50.98 1210- 815 357 989.99 2.24 12.32 814- 554 357 674.59 1.64 6.44 552- 327 357 431.92 1.25 5.32 326- 152 357 236.32 0.71 1.40 152- 20 357 81.65 0.30 0.00 19- -974 357 -133.50 -0.26 0.00 ------------------------------------------------------------------------------------ 1776012- -974 3570 43630.06 11.38 37.48 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 357 107524.59 15.06 67.23 1.64- 1.26 357 82755.19 21.80 58.54 1.26- 1.06 357 61204.62 19.38 67.23 1.06- 0.96 357 47992.09 13.32 31.65 0.96- 0.88 357 18314.93 7.54 43.14 0.88- 0.80 357 50112.74 14.03 36.41 0.80- 0.76 357 18625.99 5.80 19.05 0.76- 0.71 357 22030.31 7.12 17.65 0.71- 0.67 357 24202.31 8.02 28.57 0.67- 0.63 357 3537.79 1.78 5.32 ------------------------------------------------------------------------------------ 6.00- 0.63 3570 43630.06 11.38 37.48 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:32:46 2019 Sorting 3570 observations 43 unique observations with > 7.00 F2/sig(F2) 3570 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 49 357 Total number of frames 357 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 3570 observations in 4 runs Run # start # end # total # 1 0 11 12 2 0 11 24 3 0 11 36 4 0 5 42 Total number of frames 42 850 observations > 7.00 F2/sig(F2) 850 observations in 4 runs Run # start # end # total # 1 0 11 12 2 0 11 24 3 0 11 36 4 0 5 42 Total number of frames 42 Removing 'redundancy=1' reflections Average redundancy: 16.9 (Out of 850 removed 4 = 846, unique = 50) 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 846 observations in 4 runs Run # start # end # total # 1 0 11 12 2 0 11 24 3 0 11 36 4 0 5 42 Total number of frames 42 50 unique data precomputed (should be 50) 50 unique data with 846 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 16.9 (Out of 846 removed 0 = 846, unique = 50) 50 unique data precomputed (should be 50) 50 unique data with 846 observations RMS deviation of equivalent data = 0.24117 Rint = 0.18802 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18718, wR= 0.26043 Trying model 1 (ne=2, no=0)... Results: Rint= 0.08995, wR= 0.14272, Acormin=0.590, Acormax=1.365, Acor_av=1.012 F test: Probability=1.000, F= 4.303 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08747, wR= 0.13196, Acormin=0.503, Acormax=1.452, Acor_av=0.973 F test: Probability=0.768, F= 1.054 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08203, wR= 0.13625, Acormin=0.606, Acormax=1.465, Acor_av=1.005 F test: Probability=0.992, F= 1.189 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08168, wR= 0.12291, Acormin=0.506, Acormax=1.582, Acor_av=0.974 F test: Probability=0.525, F= 1.005 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07568, wR= 0.11447, Acormin=0.544, Acormax=1.687, Acor_av=0.981 F test: Probability=0.980, F= 1.160 Final absorption model (ne=4, no=3): Rint= 0.07568, Acormin=0.544, Acormax=1.687, Acor_av=0.981 Combined refinement in use Rint: 0.19015 There are 42 active scales (one needs to be fixed) Refinement control: frame scale #21 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 65 pars with 2145 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24117 Using Levenberg-Marquardt: 0.00010 New wR= 0.09291 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18802 with corrections 0.06515 Rint for all data: 0.19015 with corrections 0.06812 2 observations identified as outliers and rejected Cycle 2 wR= 0.08660 Using Levenberg-Marquardt: 0.00001 New wR= 0.08209 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18616 with corrections 0.05442 Rint for all data: 0.19015 with corrections 0.05868 2 observations identified as outliers and rejected Cycle 3 wR= 0.07146 Using Levenberg-Marquardt: 0.00000 New wR= 0.07031 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18489 with corrections 0.05055 Rint for all data: 0.19015 with corrections 0.05645 0 observations identified as outliers and rejected Cycle 4 wR= 0.07031 Using Levenberg-Marquardt: 0.00000 New wR= 0.07106 Using Levenberg-Marquardt: 0.00000 New wR= 0.07106 Using Levenberg-Marquardt: 0.00001 New wR= 0.07106 Using Levenberg-Marquardt: 0.00010 New wR= 0.07106 Using Levenberg-Marquardt: 0.00100 New wR= 0.07105 Using Levenberg-Marquardt: 0.01000 New wR= 0.07102 Using Levenberg-Marquardt: 0.10000 New wR= 0.07081 Using Levenberg-Marquardt: 1.00000 New wR= 0.07046 Using Levenberg-Marquardt: 10.00000 New wR= 0.07033 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18489 with corrections 0.05056 Rint for all data: 0.19015 with corrections 0.05646 Final wR= 0.07033 Final frame scales: Min= 0.8417 Max= 1.2255 Final absorption correction factors: Amin= 0.4759 Amax= 1.3966 PROFFIT INFO: Inet (after scale3 abspack): min=-963.3698 max=1177675.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=48.0707 max=24571.6250 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/103 3570 reflections read from tmp file 148 reflections are rejected (148 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 3 5 8 2 5 3 1 130 Initial Chi^2= 0.51097 Cycle 1, Chi^2= 1.01571 Current error model SIG(F2)^2 = 62.06*I_RAW + 11.08*I_BACK+(0.03635*)^2 Cycle 2, Chi^2= 1.02169 Current error model SIG(F2)^2 = 80.79*I_RAW + 6.88*I_BACK+(0.02740*)^2 Cycle 3, Chi^2= 1.01705 Current error model SIG(F2)^2 = 91.82*I_RAW + 4.80*I_BACK+(0.02374*)^2 Cycle 4, Chi^2= 1.01119 Current error model SIG(F2)^2 = 97.99*I_RAW + 3.70*I_BACK+(0.02245*)^2 Cycle 5, Chi^2= 1.00722 Current error model SIG(F2)^2 = 101.51*I_RAW + 3.07*I_BACK+(0.02199*)^2 Cycle 6, Chi^2= 1.00493 Current error model SIG(F2)^2 = 103.71*I_RAW + 2.68*I_BACK+(0.02177*)^2 Cycle 7, Chi^2= 1.00357 Current error model SIG(F2)^2 = 105.21*I_RAW + 2.41*I_BACK+(0.02163*)^2 Cycle 8, Chi^2= 1.00271 Current error model SIG(F2)^2 = 106.30*I_RAW + 2.22*I_BACK+(0.02154*)^2 Cycle 9, Chi^2= 1.00212 Current error model SIG(F2)^2 = 107.12*I_RAW + 2.07*I_BACK+(0.02148*)^2 Cycle 10, Chi^2= 1.00169 Current error model SIG(F2)^2 = 107.76*I_RAW + 1.96*I_BACK+(0.02143*)^2 Final Chi^2= 1.00169 Final error model SIG(F2)^2 = 107.76*I_RAW + 1.96*I_BACK+(0.02143*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1177676- 125500 357 383093.39 33.70 100.00 125298- 3505 357 31355.10 12.35 100.00 3502- 2005 357 2712.70 5.48 97.76 2002- 1170 357 1526.98 3.55 54.06 1170- 785 357 957.75 2.50 13.17 784- 531 357 656.71 2.14 7.00 530- 320 357 419.23 1.89 9.24 320- 156 357 232.69 1.43 2.52 155- 21 357 82.09 0.81 0.56 21- -963 357 -128.41 -0.56 0.00 ------------------------------------------------------------------------------------ 1177676- -963 3570 42090.82 6.33 38.43 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 357 104428.15 10.45 70.03 1.64- 1.26 357 80242.82 9.70 59.10 1.26- 1.06 357 61511.39 8.82 69.47 1.06- 0.96 357 44429.51 6.37 32.21 0.96- 0.88 357 18875.55 4.91 44.82 0.88- 0.80 357 46918.84 7.56 36.69 0.80- 0.76 357 17490.75 3.80 18.49 0.76- 0.71 357 20320.18 4.80 17.65 0.71- 0.67 357 23248.99 5.22 30.81 0.67- 0.63 357 3442.04 1.65 5.04 ------------------------------------------------------------------------------------ 6.00- 0.63 3570 42090.82 6.33 38.43 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 357 104428.15 10.45 70.03 6.00- 1.26 714 92335.49 10.08 64.57 6.00- 1.06 1071 82060.79 9.66 66.20 6.00- 0.96 1428 72652.97 8.84 57.70 6.00- 0.88 1785 61897.48 8.05 55.13 6.00- 0.80 2142 59401.04 7.97 52.05 6.00- 0.76 2499 53413.86 7.37 47.26 6.00- 0.71 2856 49277.15 7.05 43.56 6.00- 0.67 3213 46385.13 6.85 42.14 6.00- 0.63 3570 42090.82 6.33 38.43 ------------------------------------------------------------------------------------ 6.00- 0.63 3570 42090.82 6.33 38.43 Scale applied to data: s=0.849129 (maximum obs:1177675.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.056; Rsigma 0.035: data 3570 -> merged 162 With outlier rejection... Rint 0.053; Rsigma 0.035: data 3558 -> merged 162 Rejected total: 12, method kkm 9, method Blessing 3 Completeness direct cell (a, b, c) = (10.408, 10.408, 10.408), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626469, 6.008883 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.76 14 14 22.86 100.00 320 1.73 - 1.27 14 14 25.86 100.00 362 1.26 - 1.06 14 14 28.86 100.00 404 1.05 - 0.97 14 14 25.50 100.00 357 0.95 - 0.88 14 14 26.36 100.00 369 0.87 - 0.81 14 14 23.21 100.00 325 0.80 - 0.76 14 14 24.64 100.00 345 0.76 - 0.72 14 14 20.50 100.00 287 0.72 - 0.69 14 14 22.36 100.00 313 0.69 - 0.65 19 19 18.79 100.00 357 --------------------------------------------------------------- 7.36 - 0.65 145 145 23.72 100.00 3439 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:32:46 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.372669 7.361574 7.369788 120.1840 120.0611 89.7013 3518 Reflections read from file xs2212a.hkl 3518 Reflections used for space-group determination (up to diffraction limit of 0.47A); mean (I/sigma) = 4.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1768 1763 1765 1756 2648 2337 2346 3518 N (int>3sigma) = 0 199 203 278 192 340 534 548 795 Mean intensity = 0.0 0.9 0.9 1.3 0.9 1.0 26.9 28.9 28.0 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.5 4.9 4.7 Lattice type: P chosen Volume: 282.52 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.362 7.364 119.86 90.11 119.85 Niggli form: a.a = 53.952 b.b = 54.193 c.c = 54.235 b.c = -26.994 a.c = -0.102 a.b = -26.915 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.244 CUBIC F-lattice R(int) = 0.216 [ 3280] Vol = 1130.1 Cell: 10.391 10.446 10.411 90.07 89.85 90.09 Volume: 1130.09 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.240 RHOMBOHEDRAL R-lattice R(int) = 0.199 [ 2852] Vol = 847.6 Cell: 7.362 7.345 18.073 89.92 90.21 119.85 Volume: 847.57 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.240 RHOMBOHEDRAL R-lattice R(int) = 0.188 [ 919] Vol = 847.6 Trigonal Cell: 7.362 7.345 18.073 89.92 90.21 119.85 Volume: 847.57 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.464 TETRAGONAL I-lattice R(int) = 0.203 [ 2892] Vol = 565.0 Cell: 7.370 7.378 10.391 89.83 89.96 90.19 Volume: 565.04 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.488 TETRAGONAL I-lattice R(int) = 0.203 [ 2892] Vol = 565.0 Cell: 7.370 7.378 10.391 89.83 89.96 90.19 Volume: 565.04 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.400 ORTHORHOMBIC I-lattice R(int) = 0.171 [ 2822] Vol = 565.0 Cell: 7.370 10.391 7.378 89.83 89.81 90.04 Volume: 565.04 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.248 MONOCLINIC I-lattice R(int) = 0.169 [ 2311] Vol = 565.0 Cell: 10.391 7.370 7.378 90.19 90.17 90.04 Volume: 565.04 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.118 MONOCLINIC I-lattice R(int) = 0.159 [ 2298] Vol = 565.0 Cell: 7.364 7.345 10.446 89.99 90.11 89.89 Volume: 565.04 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.170 MONOCLINIC C-lattice R(int) = 0.165 [ 2321] Vol = 565.0 Cell: 10.391 10.446 7.345 89.99 134.87 90.09 Volume: 565.04 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) = 0.123 [ 1368] Vol = 282.5 Cell: 7.345 7.362 7.364 119.86 90.11 119.85 Volume: 282.52 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1765 0 2346 2333 3518 N (int>3sigma) = 0 0 0 0 278 0 548 543 795 Mean intensity = 0.0 0.0 0.0 0.0 1.3 0.0 28.9 29.1 28.0 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.9 4.8 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.975 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 21 21 262 674 N I>3s 0 0 0 164 0.0 0.0 -0.0 1.8 0.6 0.6 0.1 2.5 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 0.215 3046 Fd-3m 1 1 227 C N N N N 37 2284 0.217 3110 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.391493 10.445808 10.411046 90.0658 89.8502 90.0863 ZERR 1.00 0.005954 0.001006 0.010808 0.1014 0.0026 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1104689- 101086 438 431 27 16.0 334263.99 31.20 0.049 0.061 78202- 1748 663 662 27 24.5 5416.93 7.57 0.104 0.128 1668- 775 711 710 27 26.3 1157.17 2.74 0.228 0.295 703- 370 650 649 27 24.0 520.37 1.83 0.388 0.541 363- 63 588 588 27 21.8 230.09 1.29 0.538 0.821 60- -233 520 518 27 19.2 5.31 0.17 0.967 3.619 ------------------------------------------------------------------------------------------- 1104689- -233 3570 3558 162 22.0 41863.73 6.31 0.053 0.066 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-1.27 681 680 27 25.2 95994.70 10.46 0.048 0.059 0.025 1.26-0.97 763 761 28 27.2 49493.85 7.17 0.047 0.062 0.032 0.95-0.81 696 694 28 24.8 33733.33 6.37 0.057 0.072 0.042 0.80-0.73 618 615 27 22.8 17544.14 4.06 0.058 0.063 0.056 0.72-0.67 543 540 27 20.0 19679.12 4.56 0.080 0.105 0.064 0.66-0.63 269 268 25 10.7 4412.80 1.83 0.164 0.100 0.123 ------------------------------------------------------------------------------------------------------ inf-0.63 3570 3558 162 22.0 41863.73 6.31 0.053 0.066 0.035 inf-0.65 3448 3437 144 23.9 43077.30 6.45 0.052 0.064 0.035 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-1.27 680 27 27 100.0 25.2 95994.70 49.86 0.048 0.007 1.26-0.97 761 28 28 100.0 27.2 49493.85 35.04 0.047 0.008 0.95-0.81 694 28 28 100.0 24.8 33733.33 32.18 0.057 0.010 0.80-0.73 615 27 27 100.0 22.8 17544.14 17.60 0.058 0.014 0.72-0.67 540 27 27 100.0 20.0 19679.12 22.20 0.080 0.015 0.66-0.63 268 25 25 100.0 10.7 4412.80 6.34 0.164 0.042 -------------------------------------------------------------------------------------------- inf-0.63 3558 162 162 100.0 22.0 41863.73 30.19 0.053 0.010 inf-0.65 3437 144 144 100.0 23.9 43077.30 31.06 0.052 0.009 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:39:19 2019) ID: 3668; threads 40; handles 809; mem 515336.00 (1204688.00)kB; time: 1w 4d 23h 50m 7s MEMORY INFO: Memory PF:279.0, Ph:625.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:503.3,peak PF: 700.2, WS: 471.3, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:281.0, Ph:627.0, V:1178.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:505.1,peak PF: 700.2, WS: 473.1, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:39:19 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000089 0.000065 0.000091 ) 0.064809 0.092374 0.027273 ( 0.000109 0.000079 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000131 0.000096 0.000134 ) 7.38096 ( 0.00697 ) 7.36649 ( 0.00759 ) 7.42630 ( 0.00886 ) 120.52449 ( 0.11837 ) 120.40327 ( 0.11361 ) 89.27095 ( 0.07996 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:39:19 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000089 0.000065 0.000091 ) 0.064809 0.092374 0.027273 ( 0.000109 0.000079 0.000111 ) 0.045523 0.057900 0.132205 ( 0.000131 0.000096 0.000134 ) M - matrix: 0.013765 0.004541 0.009165 ( 0.000024 0.000016 0.000021 ) 0.004541 0.013984 0.009352 ( 0.000016 0.000019 0.000019 ) 0.009165 0.009352 0.018539 ( 0.000021 0.000019 0.000036 ) unit cell: 7.381(7) 7.366(8) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.82 | 24 | 1.005 ( 0.047) | 1.008 ( 0.130) | 0.907 ( 0.354) | 0.79- 0.69 | 24 | 0.998 ( 0.044) | 1.006 ( 0.137) | 1.289 ( 0.497) | 0.69- 0.63 | 23 | 0.979 ( 0.051) | 0.913 ( 0.103) | 1.157 ( 0.432) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.510) | 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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb PROFFITPEAK info: 299 peaks in the peak location table UB fit with 31 obs out of 162 (total:162,skipped:0) (19.14%) UB - matrix: 0.085696 -0.045820 0.016935 ( 0.000638 0.000186 0.000313 ) 0.064725 0.092564 0.027613 ( 0.000794 0.000232 0.000390 ) 0.045992 0.058003 0.132873 ( 0.001278 0.000373 0.000627 ) M - matrix: 0.013648 0.004732 0.009350 ( 0.000191 0.000112 0.000178 ) 0.004732 0.014032 0.009487 ( 0.000112 0.000063 0.000073 ) 0.009350 0.009487 0.018704 ( 0.000178 0.000073 0.000168 ) unit cell: 7.49(4) 7.39(4) 7.41(5) 120.4(7) 120.4(7) 89.9(5) V = 287(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 4, #refl in peak table: 162 #indexed refl 147, indexation with best UB: 90.7407% Lattice: 7.4226 7.3563 7.3586 120.029 120.251 89.813 283.374 Rotation: -22.685 24.746 -35.046 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 157 obs out of 162 (total:162,skipped:0) (96.91%) UB - matrix: 0.087732 -0.044390 0.012620 ( 0.000092 0.000072 0.000074 ) 0.061560 0.094363 0.026224 ( 0.000097 0.000077 0.000079 ) 0.049340 0.055535 0.133299 ( 0.000086 0.000068 0.000069 ) M - matrix: 0.013921 0.004655 0.009298 ( 0.000022 0.000014 0.000015 ) 0.004655 0.013959 0.009317 ( 0.000014 0.000018 0.000013 ) 0.009298 0.009317 0.018616 ( 0.000015 0.000013 0.000019 ) unit cell: 7.364(7) 7.357(7) 7.356(5) 120.03(9) 120.00(8) 90.00(7) V = 281.7(4) OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 UB - matrix: 0.087891 -0.044289 0.012621 ( 0.000088 0.000071 0.000073 ) 0.061598 0.094450 0.026164 ( 0.000096 0.000077 0.000079 ) 0.049404 0.055532 0.133170 ( 0.000086 0.000069 0.000071 ) M - matrix: 0.013960 0.004669 0.009300 ( 0.000021 0.000014 0.000015 ) 0.004669 0.013966 0.009307 ( 0.000014 0.000018 0.000013 ) 0.009300 0.009307 0.018578 ( 0.000015 0.000013 0.000019 ) UB fit with 159 obs out of 162 (total:162,skipped:0) (98.15%) unit cell: 7.353(6) 7.354(7) 7.360(5) 120.00(9) 119.97(8) 90.06(7) V = 281.4(4) UB fit with 159 obs out of 162 (total:162,skipped:0) (98.15%) UB - matrix: 0.087891 -0.044289 0.012621 ( 0.000088 0.000071 0.000073 ) 0.061598 0.094450 0.026164 ( 0.000096 0.000077 0.000079 ) 0.049404 0.055532 0.133170 ( 0.000086 0.000069 0.000071 ) M - matrix: 0.013960 0.004669 0.009300 ( 0.000021 0.000014 0.000015 ) 0.004669 0.013966 0.009307 ( 0.000014 0.000018 0.000013 ) 0.009300 0.009307 0.018578 ( 0.000015 0.000013 0.000019 ) unit cell: 7.353(6) 7.354(7) 7.360(5) 120.00(9) 119.97(8) 90.06(7) V = 281.4(4) OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 UB - matrix: 0.087891 -0.044289 0.012621 ( 0.000088 0.000071 0.000073 ) 0.061598 0.094450 0.026164 ( 0.000096 0.000077 0.000079 ) 0.049404 0.055532 0.133170 ( 0.000086 0.000069 0.000071 ) M - matrix: 0.013960 0.004669 0.009300 ( 0.000021 0.000014 0.000015 ) 0.004669 0.013966 0.009307 ( 0.000014 0.000018 0.000013 ) 0.009300 0.009307 0.018578 ( 0.000015 0.000013 0.000019 ) UB fit with 159 obs out of 162 (total:162,skipped:0) (98.15%) unit cell: 7.353(6) 7.354(7) 7.360(5) 120.00(9) 119.97(8) 90.06(7) V = 281.4(4) 162 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Run 4 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1007 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087891 -0.044289 0.012621 ( 0.000088 0.000071 0.000073 ) 0.061598 0.094450 0.026164 ( 0.000096 0.000077 0.000079 ) 0.049404 0.055532 0.133170 ( 0.000086 0.000069 0.000071 ) M - matrix: 0.013960 0.004669 0.009300 ( 0.000021 0.000014 0.000015 ) 0.004669 0.013966 0.009307 ( 0.000014 0.000018 0.000013 ) 0.009300 0.009307 0.018578 ( 0.000015 0.000013 0.000019 ) UB fit with 159 obs out of 162 (total:162,skipped:0) (98.15%) unit cell: 7.353(6) 7.354(7) 7.360(5) 120.00(9) 119.97(8) 90.06(7) V = 281.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 159 obs out of 162 (total:162,skipped:0) (98.15%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb 0 of 154 peaks identified as outliers and rejected 154 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 154 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 154 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.60 | 15 | 0.881 ( 0.095) | 0.891 ( 0.129) | 0.909 ( 0.477) | 2.57- 1.83 | 15 | 0.879 ( 0.106) | 0.902 ( 0.137) | 0.871 ( 0.222) | 1.82- 1.57 | 15 | 0.861 ( 0.122) | 0.867 ( 0.162) | 0.848 ( 0.364) | 1.57- 1.36 | 15 | 0.960 ( 0.084) | 0.985 ( 0.131) | 0.799 ( 0.335) | 1.35- 1.19 | 15 | 0.923 ( 0.087) | 0.939 ( 0.113) | 0.851 ( 0.469) | 1.19- 1.00 | 15 | 0.963 ( 0.083) | 0.979 ( 0.123) | 0.875 ( 0.312) | 1.00- 0.88 | 15 | 0.989 ( 0.070) | 0.981 ( 0.080) | 1.035 ( 0.343) | 0.88- 0.82 | 15 | 0.995 ( 0.045) | 0.979 ( 0.127) | 0.998 ( 0.348) | 0.79- 0.72 | 15 | 0.965 ( 0.042) | 0.935 ( 0.081) | 1.363 ( 0.483) | 0.69- 0.63 | 19 | 0.958 ( 0.047) | 0.907 ( 0.084) | 1.223 ( 0.450) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 154 | 0.938 ( 0.093) | 0.936 ( 0.126) | 0.984 ( 0.429) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 154 obs out of 154 (total:154,skipped:0) (100.00%) UB - matrix: 0.088067 -0.044257 0.012886 ( 0.000046 0.000039 0.000039 ) 0.061453 0.094509 0.026030 ( 0.000039 0.000033 0.000033 ) 0.049292 0.055416 0.133118 ( 0.000029 0.000025 0.000025 ) M - matrix: 0.013962 0.004642 0.009296 ( 0.000010 0.000006 0.000006 ) 0.004642 0.013962 0.009267 ( 0.000006 0.000008 0.000005 ) 0.009296 0.009267 0.018564 ( 0.000006 0.000005 0.000007 ) unit cell: 7.352(3) 7.341(3) 7.354(2) 119.88(4) 120.04(4) 90.01(3) V = 280.98(18) OTKP changes: 154 1 1 1 OTKP changes: 154 1 1 1 OTKP changes: 154 1 1 1 UB - matrix: 0.087871 -0.044360 0.012691 ( 0.000036 0.000031 0.000031 ) 0.061542 0.094401 0.026168 ( 0.000031 0.000027 0.000027 ) 0.049368 0.055469 0.133225 ( 0.000027 0.000023 0.000023 ) M - matrix: 0.013946 0.004650 0.009303 ( 0.000008 0.000005 0.000005 ) 0.004650 0.013956 0.009297 ( 0.000005 0.000006 0.000004 ) 0.009303 0.009297 0.018595 ( 0.000005 0.000004 0.000006 ) UB fit with 154 obs out of 154 (total:154,skipped:0) (100.00%) unit cell: 7.358(2) 7.352(2) 7.3569(18) 119.98(3) 120.03(3) 89.99(3) V = 281.40(15) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1006 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087871 -0.044360 0.012691 ( 0.000036 0.000031 0.000031 ) 0.061542 0.094401 0.026168 ( 0.000031 0.000027 0.000027 ) 0.049368 0.055469 0.133225 ( 0.000027 0.000023 0.000023 ) M - matrix: 0.013946 0.004650 0.009303 ( 0.000008 0.000005 0.000005 ) 0.004650 0.013956 0.009297 ( 0.000005 0.000006 0.000004 ) 0.009303 0.009297 0.018595 ( 0.000005 0.000004 0.000006 ) UB fit with 154 obs out of 154 (total:154,skipped:0) (100.00%) unit cell: 7.358(2) 7.352(2) 7.3569(18) 119.98(3) 120.03(3) 89.99(3) V = 281.40(15) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 154 obs out of 154 (total:154,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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb 0 of 152 peaks identified as outliers and rejected 152 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 152 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 152 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 2.59 | 15 | 0.875 ( 0.105) | 0.886 ( 0.134) | 0.952 ( 0.442) | 2.39- 1.83 | 15 | 0.880 ( 0.107) | 0.903 ( 0.136) | 0.934 ( 0.315) | 1.76- 1.57 | 15 | 0.854 ( 0.122) | 0.863 ( 0.170) | 0.767 ( 0.287) | 1.56- 1.36 | 15 | 0.960 ( 0.084) | 0.982 ( 0.130) | 0.808 ( 0.334) | 1.35- 1.19 | 15 | 0.928 ( 0.085) | 0.953 ( 0.106) | 0.787 ( 0.463) | 1.19- 1.00 | 15 | 0.971 ( 0.086) | 0.980 ( 0.128) | 0.884 ( 0.306) | 1.00- 0.88 | 15 | 0.983 ( 0.070) | 1.013 ( 0.086) | 0.960 ( 0.300) | 0.88- 0.79 | 15 | 0.993 ( 0.044) | 0.959 ( 0.113) | 1.110 ( 0.418) | 0.79- 0.69 | 15 | 0.968 ( 0.047) | 0.949 ( 0.094) | 1.258 ( 0.502) | 0.69- 0.63 | 17 | 0.950 ( 0.042) | 0.887 ( 0.066) | 1.273 ( 0.448) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 0.63 | 152 | 0.936 ( 0.095) | 0.937 ( 0.128) | 0.977 ( 0.428) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 86 | 0.982 ( 0.036) | 1.029 ( 0.071) | 1.112 ( 0.490) | 10.4-14.9 | 86 | 0.982 ( 0.043) | 1.038 ( 0.069) | 1.203 ( 0.568) | 14.9-19.1 | 86 | 0.994 ( 0.227) | 1.023 ( 0.098) | 1.214 ( 1.163) | 19.2-23.6 | 86 | 0.955 ( 0.056) | 0.996 ( 0.082) | 0.927 ( 0.429) | 23.6-27.5 | 86 | 0.959 ( 0.065) | 0.993 ( 0.098) | 0.930 ( 0.411) | 27.5-32.7 | 86 | 0.944 ( 0.086) | 0.952 ( 0.109) | 0.952 ( 0.464) | 32.8-36.4 | 86 | 0.916 ( 0.167) | 0.898 ( 0.135) | 1.086 ( 0.669) | 36.4-39.0 | 86 | 0.875 ( 0.093) | 0.844 ( 0.125) | 1.012 ( 0.500) | 39.0-42.0 | 86 | 0.893 ( 0.096) | 0.839 ( 0.126) | 1.047 ( 0.485) | 42.1-50.1 | 83 | 0.876 ( 0.120) | 0.802 ( 0.137) | 0.956 ( 0.459) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 857 | 0.938 ( 0.121) | 0.942 ( 0.136) | 1.044 ( 0.611) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.13 e2 dimension: a=-0.0070 b=1.24 e3 dimension: a=0.0007 b=1.08 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3814 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:39:32 2019 PROFFITMAIN - Started at Wed Aug 21 13:39:32 2019 OTKP changes: 334 2 3 4 OTKP changes: 334 2 3 4 OTKP changes: 334 2 3 4 UB - matrix: 0.087683 -0.045997 0.016764 ( 0.000085 0.000065 0.000086 ) 0.063250 0.092388 0.026771 ( 0.000096 0.000073 0.000096 ) 0.045280 0.057594 0.131912 ( 0.000098 0.000075 0.000099 ) M - matrix: 0.013739 0.004418 0.009136 ( 0.000021 0.000014 0.000017 ) 0.004418 0.013968 0.009300 ( 0.000014 0.000017 0.000015 ) 0.009136 0.009300 0.018399 ( 0.000017 0.000015 0.000027 ) UB fit with 384 obs out of 857 (total:857,skipped:0) (44.81%) unit cell: 7.396(6) 7.370(7) 7.436(7) 120.77(10) 120.31(9) 88.76(7) V = 284.9(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) UB - matrix: 0.087605 -0.046161 0.017191 ( 0.000107 0.000066 0.000100 ) 0.064581 0.092364 0.027082 ( 0.000091 0.000056 0.000085 ) 0.045798 0.057746 0.132031 ( 0.000108 0.000067 0.000102 ) M - matrix: 0.013943 0.004566 0.009302 ( 0.000024 0.000014 0.000018 ) 0.004566 0.013997 0.009332 ( 0.000014 0.000014 0.000014 ) 0.009302 0.009332 0.018461 ( 0.000018 0.000014 0.000027 ) unit cell: 7.373(7) 7.364(7) 7.438(7) 120.52(10) 120.45(10) 89.16(7) V = 283.4(4) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.175) HKL list info: 1284 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087480 -0.046173 0.017357 ( 0.000100 0.000062 0.000093 ) 0.064777 0.092358 0.027258 ( 0.000086 0.000053 0.000080 ) 0.045689 0.057810 0.132113 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013936 0.004585 0.009320 ( 0.000023 0.000013 0.000018 ) 0.004585 0.014004 0.009354 ( 0.000013 0.000014 0.000013 ) 0.009320 0.009354 0.018498 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.379(6) 7.366(6) 7.435(6) 120.52(9) 120.47(9) 89.21(7) V = 283.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 204 obs out of 212 (total:212,skipped:0) (96.23%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.117980 0.038997 0.078622 ( 0.000076 0.000047 0.000070 ) 0.000082 0.111534 0.056278 ( 0.000080 0.000050 0.000074 ) -0.000026 -0.000077 0.095364 ( 0.000089 0.000056 0.000083 ) M - matrix: 0.013919 0.004610 0.009278 ( 0.000018 0.000011 0.000014 ) 0.004610 0.013961 0.009336 ( 0.000011 0.000012 0.000011 ) 0.009278 0.009336 0.018443 ( 0.000014 0.000011 0.000021 ) UB fit with 207 obs out of 212 (total:212,skipped:0) (97.64%) unit cell: 7.375(5) 7.381(5) 7.434(8) 120.48(9) 120.25(9) 89.46(6) V = 284.3(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.087804 -0.044309 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094149 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055798 0.133161 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004658 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009312 0.018585 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3551(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 152 obs out of 152 (total:152,skipped:0) (100.00%) UB - matrix: 0.087874 -0.044365 0.012695 ( 0.000038 0.000032 0.000032 ) 0.061531 0.094402 0.026159 ( 0.000032 0.000027 0.000027 ) 0.049378 0.055450 0.133213 ( 0.000026 0.000022 0.000022 ) M - matrix: 0.013946 0.004648 0.009303 ( 0.000008 0.000005 0.000005 ) 0.004648 0.013955 0.009293 ( 0.000005 0.000006 0.000004 ) 0.009303 0.009293 0.018591 ( 0.000005 0.000004 0.000006 ) unit cell: 7.359(3) 7.351(2) 7.3572(17) 119.97(3) 120.04(3) 89.99(3) V = 281.41(15) OTKP changes: 152 1 1 1 OTKP changes: 152 1 1 1 OTKP changes: 152 1 1 1 OTKP changes: 152 1 1 1 OTKP changes: 152 1 1 1 OTKP changes: 152 1 1 1 Run 4 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 984 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087874 -0.044365 0.012695 ( 0.000038 0.000032 0.000032 ) 0.061531 0.094402 0.026159 ( 0.000032 0.000027 0.000027 ) 0.049378 0.055450 0.133213 ( 0.000026 0.000022 0.000022 ) M - matrix: 0.013946 0.004648 0.009303 ( 0.000008 0.000005 0.000005 ) 0.004648 0.013955 0.009293 ( 0.000005 0.000006 0.000004 ) 0.009303 0.009293 0.018591 ( 0.000005 0.000004 0.000006 ) UB fit with 152 obs out of 152 (total:152,skipped:0) (100.00%) unit cell: 7.359(3) 7.351(2) 7.3572(17) 119.97(3) 120.04(3) 89.99(3) V = 281.41(15) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 152 obs out of 152 (total:152,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: 0.087874 -0.044365 0.012695 ( 0.000038 0.000032 0.000032 ) 0.061531 0.094402 0.026159 ( 0.000032 0.000027 0.000027 ) 0.049378 0.055450 0.133213 ( 0.000026 0.000022 0.000022 ) M - matrix: 0.013946 0.004648 0.009303 ( 0.000008 0.000005 0.000005 ) 0.004648 0.013955 0.009293 ( 0.000005 0.000006 0.000004 ) 0.009303 0.009293 0.018591 ( 0.000005 0.000004 0.000006 ) UB fit with 152 obs out of 152 (total:152,skipped:0) (100.00%) unit cell: 7.359(3) 7.351(2) 7.3572(17) 119.97(3) 120.04(3) 89.99(3) V = 281.41(15) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 68.89 ph= 0.28 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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117670 0.038695 0.078476 ( 0.000041 0.000039 0.000044 ) 0.000019 0.111489 0.056080 ( 0.000028 0.000026 0.000030 ) -0.000065 -0.000139 0.096136 ( 0.000030 0.000028 0.000033 ) M - matrix: 0.013846 0.004555 0.009229 ( 0.000010 0.000006 0.000007 ) 0.004555 0.013927 0.009275 ( 0.000006 0.000007 0.000006 ) 0.009229 0.009275 0.018546 ( 0.000007 0.000006 0.000010 ) UB fit with 850 obs out of 857 (total:857,skipped:0) (99.18%) unit cell: 7.374(3) 7.360(2) 7.370(3) 120.18(4) 120.08(4) 89.63(3) V = 282.66(17) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 85 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof 3831 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:39:38 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.175) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-565.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-588.7455 max=1111814.4646 PROFFIT INFO: background sum: min=-42.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=412.0000 max=5617.0000 PROFFIT INFO: num of signal pixels: min=41 max=497 PROFFIT INFO: Inet: min=-941.9929 max=1778903.2500 PROFFIT INFO: sig(Inet): min=57.5968 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.72 max=198.39 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 349 1351 2016 2406 2575 2992 3235 3388 3640 3789 3831 Percent 9.1 35.3 52.6 62.8 67.2 78.1 84.4 88.4 95.0 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3831 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 3831 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1778903- 126780 383 389443.27 76.08 100.00 126205- 3859 383 29071.80 19.45 100.00 3859- 2002 383 2774.99 6.85 97.13 1997- 1174 383 1534.09 3.83 50.39 1174- 788 383 967.44 2.22 11.75 786- 521 383 649.32 1.64 7.05 519- 317 383 411.65 1.19 4.70 316- 143 383 226.73 0.67 1.04 143- 10 383 73.84 0.27 0.00 10- -942 384 -132.06 -0.26 0.00 ------------------------------------------------------------------------------------ 1778903- -942 3831 42490.98 11.19 37.20 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 383 93617.08 16.00 68.93 1.75- 1.26 383 92299.79 21.95 57.96 1.26- 1.02 383 55774.16 16.19 51.17 1.02- 0.90 383 33461.44 10.26 38.12 0.90- 0.81 383 26949.26 8.77 31.33 0.81- 0.73 383 42111.53 12.51 40.21 0.73- 0.68 383 21469.94 7.03 24.02 0.68- 0.61 383 23704.47 7.41 24.02 0.61- 0.56 383 20512.85 6.67 19.84 0.56- 0.44 384 15080.82 5.13 16.41 ------------------------------------------------------------------------------------ 6.55- 0.44 3831 42490.98 11.19 37.20 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:39:38 2019 Sorting 3831 observations 88 unique observations with > 7.00 F2/sig(F2) 3831 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 74 382 Total number of frames 382 Maximum number of 88 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 3831 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 14 78 Total number of frames 78 904 observations > 7.00 F2/sig(F2) 904 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 14 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 7.1 (Out of 904 removed 33 = 871, unique = 123) 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 871 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 14 78 Total number of frames 78 123 unique data precomputed (should be 123) 123 unique data with 871 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.1 (Out of 871 removed 0 = 871, unique = 123) 123 unique data precomputed (should be 123) 123 unique data with 871 observations RMS deviation of equivalent data = 0.39061 Rint = 0.35003 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.34923, wR= 0.47158 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26057, wR= 0.35444, Acormin=0.543, Acormax=1.464, Acor_av=1.023 F test: Probability=1.000, F= 1.784 Trying model 2 (ne=2, no=1)... Results: Rint= 0.25418, wR= 0.34981, Acormin=0.531, Acormax=1.495, Acor_av=0.977 F test: Probability=0.732, F= 1.047 Trying model 3 (ne=4, no=0)... Results: Rint= 0.25933, wR= 0.35021, Acormin=0.505, Acormax=1.590, Acor_av=0.975 F test: Probability=0.000, F= 0.997 Trying model 4 (ne=4, no=1)... Results: Rint= 0.24761, wR= 0.34205, Acormin=0.397, Acormax=1.627, Acor_av=0.945 F test: Probability=0.877, F= 1.090 Trying model 5 (ne=4, no=3)... Results: Rint= 0.24189, wR= 0.32267, Acormin=0.292, Acormax=1.748, Acor_av=0.866 F test: Probability=0.952, F= 1.131 Trying model 6 (ne=6, no=0)... Results: Rint= 0.25461, wR= 0.33201, Acormin=0.219, Acormax=1.634, Acor_av=0.927 F test: Probability=0.000, F= 0.899 Trying model 7 (ne=6, no=1)... Results: Rint= 0.24269, wR= 0.32002, Acormin=0.225, Acormax=1.698, Acor_av=0.927 F test: Probability=0.000, F= 0.985 Trying model 8 (ne=6, no=3)... Results: Rint= 0.24525, wR= 0.31261, Acormin=0.167, Acormax=1.808, Acor_av=0.822 F test: Probability=0.000, F= 0.955 Trying model 9 (ne=6, no=5)... Results: Rint= 0.25325, wR= 0.32051, Acormin=0.165, Acormax=2.021, Acor_av=0.748 F test: Probability=0.000, F= 0.882 Trying model 10 (ne=8, no=0)... Results: Rint= 0.26510, wR= 0.32486, Acormin=-0.021, Acormax=1.629, Acor_av=0.842 F test: Probability=0.000, F= 0.810 Trying model 11 (ne=8, no=1)... Results: Rint= 0.31024, wR= 0.36859, Acormin=-0.001, Acormax=1.330, Acor_av=0.607 F test: Probability=0.000, F= 0.589 Trying model 12 (ne=8, no=3)... Results: Rint= 0.32808, wR= 0.37972, Acormin=-0.002, Acormax=0.110, Acor_av=0.038 F test: Probability=0.000, F= 0.521 Trying model 13 (ne=8, no=5)... Results: Rint= 0.29182, wR= 0.35001, Acormin=-0.004, Acormax=0.106, Acor_av=0.042 F test: Probability=0.000, F= 0.648 Trying model 14 (ne=8, no=7)... Results: Rint= 0.23536, wR= 0.30166, Acormin=-0.017, Acormax=0.157, Acor_av=0.044 F test: Probability=0.000, F= 0.974 Final absorption model (ne=4, no=3): Rint= 0.24189, Acormin=0.292, Acormax=1.748, Acor_av=0.866 Combined refinement in use Rint: 0.36437 There are 78 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 101 pars with 5151 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.39061 Using Levenberg-Marquardt: 0.00010 New wR= 0.20883 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35003 with corrections 0.18015 Rint for all data: 0.36437 with corrections 0.19671 1 observations identified as outliers and rejected Cycle 2 wR= 0.20348 Using Levenberg-Marquardt: 0.00001 New wR= 0.19307 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34967 with corrections 0.16558 Rint for all data: 0.36437 with corrections 0.18472 0 observations identified as outliers and rejected Cycle 3 wR= 0.19307 Using Levenberg-Marquardt: 0.00000 New wR= 0.19198 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34967 with corrections 0.16399 Rint for all data: 0.36437 with corrections 0.18290 0 observations identified as outliers and rejected Cycle 4 wR= 0.19198 Using Levenberg-Marquardt: 0.00000 New wR= 0.19325 Using Levenberg-Marquardt: 0.00000 New wR= 0.19325 Using Levenberg-Marquardt: 0.00001 New wR= 0.19324 Using Levenberg-Marquardt: 0.00010 New wR= 0.19322 Using Levenberg-Marquardt: 0.00100 New wR= 0.19300 Using Levenberg-Marquardt: 0.01000 New wR= 0.19158 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34967 with corrections 0.16345 Rint for all data: 0.36437 with corrections 0.18227 0 observations identified as outliers and rejected Cycle 5 wR= 0.19158 Using Levenberg-Marquardt: 0.00100 New wR= 0.19436 Using Levenberg-Marquardt: 0.01000 New wR= 0.19265 Using Levenberg-Marquardt: 0.10000 New wR= 0.19024 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.34967 with corrections 0.16189 Rint for all data: 0.36437 with corrections 0.18069 0 observations identified as outliers and rejected Final wR= 0.19024 Final frame scales: Min= 0.7365 Max= 2.8997 Final absorption correction factors: Amin= 0.1238 Amax= 1.7308 PROFFIT INFO: Inet (after scale3 abspack): min=-2095.2246 max=1277033.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=45.0034 max=27590.7773 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/103 3831 reflections read from tmp file 941 reflections are rejected (888 as outliers, 53 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 79 57 33 41 37 29 19 22 110 Initial Chi^2= 2.16688 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.86640 Current error model SIG(F2)^2 = 460.12*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 398.65*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 398.65*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1277034- 113396 383 347041.26 32.23 100.00 111711- 3652 383 25273.66 6.87 82.25 3646- 1865 383 2513.06 2.68 29.50 1864- 1095 383 1449.47 1.98 15.93 1093- 696 383 878.56 1.40 2.09 694- 459 383 572.29 1.14 0.26 459- 277 383 364.62 1.01 0.52 276- 129 383 203.17 0.83 0.52 129- 9 383 66.92 0.48 0.26 9- -2095 384 -153.11 -0.35 0.00 ------------------------------------------------------------------------------------ 1277034- -2095 3831 37811.08 4.83 23.13 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 383 87884.23 10.91 52.74 1.75- 1.26 383 86103.16 9.37 39.95 1.26- 1.02 383 52484.28 6.31 33.42 1.02- 0.90 383 29762.83 3.82 16.45 0.90- 0.81 383 24169.69 3.32 13.84 0.81- 0.73 383 36504.75 4.48 22.45 0.73- 0.68 383 17900.61 2.70 11.75 0.68- 0.61 383 18357.37 2.80 13.58 0.61- 0.56 383 15283.78 2.54 15.40 0.56- 0.44 384 9733.38 2.02 11.72 ------------------------------------------------------------------------------------ 6.55- 0.44 3831 37811.08 4.83 23.13 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 383 87884.23 10.91 52.74 6.55- 1.26 766 86993.69 10.14 46.34 6.55- 1.02 1149 75490.56 8.86 42.04 6.55- 0.90 1532 64058.62 7.60 35.64 6.55- 0.81 1915 56080.84 6.75 31.28 6.55- 0.73 2298 52818.16 6.37 29.81 6.55- 0.68 2681 47829.93 5.84 27.23 6.55- 0.61 3064 44145.86 5.46 25.52 6.55- 0.56 3447 40938.97 5.14 24.40 6.55- 0.44 3831 37811.08 4.83 23.13 ------------------------------------------------------------------------------------ 6.55- 0.44 3831 37811.08 4.83 23.13 Scale applied to data: s=0.783064 (maximum obs:1277033.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.181; Rsigma 0.050: data 3831 -> merged 485 With outlier rejection... Rint 0.174; Rsigma 0.050: data 3778 -> merged 485 Rejected total: 53, method kkm 44, method Blessing 9 Completeness direct cell (a, b, c) = (6.563, 6.563, 6.563), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445511, 6.562791 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.59 22 22 20.23 100.00 445 1.55 - 1.22 22 22 17.86 100.00 393 1.20 - 1.02 22 22 15.32 100.00 337 1.02 - 0.92 22 22 13.05 100.00 287 0.92 - 0.84 22 22 13.18 100.00 290 0.84 - 0.79 22 22 10.27 100.00 226 0.79 - 0.75 22 22 10.95 100.00 241 0.75 - 0.71 22 22 8.36 100.00 184 0.71 - 0.69 22 22 8.73 100.00 192 0.68 - 0.65 26 29 8.54 89.66 222 --------------------------------------------------------------- 7.36 - 0.65 224 227 12.58 98.68 2817 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:39:39 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.373727 7.360010 7.370202 120.1791 120.0756 89.6258 3778 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.79 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1890 1891 1897 1882 2839 2516 2522 3778 N (int>3sigma) = 0 210 228 306 213 372 588 595 865 Mean intensity = 0.0 0.9 0.9 1.3 0.9 1.0 28.7 30.2 29.4 Mean int/sigma = 0.0 1.4 1.5 1.9 1.4 1.6 4.7 4.9 4.8 Lattice type: P chosen Volume: 282.66 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.360 7.364 119.78 90.18 119.84 Niggli form: a.a = 53.951 b.b = 54.170 c.c = 54.222 b.c = -26.915 a.c = -0.170 a.b = -26.901 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.297 CUBIC F-lattice R(int) = 0.237 [ 3541] Vol = 1130.6 Cell: 10.384 10.452 10.417 90.13 89.86 90.11 Volume: 1130.64 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.292 RHOMBOHEDRAL R-lattice R(int) = 0.219 [ 3106] Vol = 848.0 Cell: 7.360 7.345 18.084 89.84 90.30 119.84 Volume: 847.98 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.292 RHOMBOHEDRAL R-lattice R(int) = 0.228 [ 1005] Vol = 848.0 Trigonal Cell: 7.360 7.345 18.084 89.84 90.30 119.84 Volume: 847.98 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.496 TETRAGONAL I-lattice R(int) = 0.226 [ 3154] Vol = 565.3 Cell: 7.370 7.387 10.384 89.82 89.97 90.19 Volume: 565.32 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.491 TETRAGONAL I-lattice R(int) = 0.226 [ 3154] Vol = 565.3 Cell: 7.370 7.387 10.384 89.82 89.97 90.19 Volume: 565.32 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.378 ORTHORHOMBIC I-lattice R(int) = 0.191 [ 3081] Vol = 565.3 Cell: 7.370 10.384 7.387 89.82 89.81 90.03 Volume: 565.32 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.226 MONOCLINIC I-lattice R(int) = 0.187 [ 2565] Vol = 565.3 Cell: 10.384 7.370 7.387 90.19 90.18 90.03 Volume: 565.32 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.186 MONOCLINIC I-lattice R(int) = 0.161 [ 2553] Vol = 565.3 Cell: 7.364 7.345 10.452 90.01 90.17 89.82 Volume: 565.32 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.220 MONOCLINIC C-lattice R(int) = 0.173 [ 2578] Vol = 565.3 Cell: 10.384 10.452 7.345 90.01 134.84 90.11 Volume: 565.32 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) = 0.111 [ 1616] Vol = 282.7 Cell: 7.345 7.360 7.364 119.78 90.18 119.84 Volume: 282.66 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1897 0 2522 2506 3778 N (int>3sigma) = 0 0 0 0 306 0 595 586 865 Mean intensity = 0.0 0.0 0.0 0.0 1.3 0.0 30.2 29.7 29.4 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.9 4.8 4.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.978 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 26 26 285 724 N I>3s 0 0 0 180 0.0 0.0 -0.0 1.8 0.5 0.5 0.1 2.5 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 0.237 3284 Fd-3m 1 1 227 C N N N N 37 2284 0.236 3348 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.384253 10.452295 10.416986 90.1275 89.8568 90.1067 ZERR 1.00 0.005959 0.000998 0.010789 0.0997 0.0031 0.0049 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 810586- 90251 420 406 48 8.5 329112.69 30.76 0.156 0.171 87995- 2410 493 486 48 10.1 11556.31 4.25 0.318 0.171 2405- 1384 631 622 48 13.0 1894.55 2.18 0.835 0.940 1383- 936 585 580 48 12.1 1064.42 1.40 0.782 0.913 933- 727 375 372 48 7.8 827.08 1.20 0.645 0.656 726- 545 396 387 48 8.1 577.46 0.94 0.731 0.832 542- 420 283 281 48 5.9 481.87 0.86 0.644 0.675 418- 285 250 248 48 5.2 367.60 0.71 0.706 0.863 283- 128 241 240 48 5.0 197.47 0.48 0.864 1.318 127- -335 157 156 53 2.9 26.24 0.15 0.969 2.621 ------------------------------------------------------------------------------------------- 810586- -335 3831 3778 485 7.8 37543.97 4.79 0.174 0.183 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-1.14 936 926 49 18.9 76705.56 9.08 0.194 0.218 0.027 1.13-0.89 685 678 50 13.6 38608.48 4.73 0.154 0.171 0.053 0.88-0.76 549 543 49 11.1 33595.72 4.13 0.155 0.183 0.070 0.76-0.69 438 433 48 9.0 25005.54 3.43 0.152 0.167 0.077 0.69-0.63 383 380 51 7.5 18099.68 2.79 0.180 0.187 0.095 0.63-0.58 300 291 50 5.8 10167.21 1.96 0.208 0.214 0.120 0.58-0.55 207 199 49 4.1 16846.66 2.80 0.087 0.087 0.103 0.55-0.52 142 141 48 2.9 4040.68 1.27 0.108 0.116 0.205 0.52-0.49 120 117 48 2.4 12812.17 2.44 0.082 0.084 0.112 0.49-0.45 71 70 43 1.6 4393.57 1.20 0.417 0.487 0.186 ------------------------------------------------------------------------------------------------------ inf-0.45 3831 3778 485 7.8 37543.97 4.79 0.174 0.183 0.050 inf-0.65 2847 2817 224 12.6 45788.22 5.62 0.177 0.195 0.044 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-1.14 926 49 49 100.0 18.9 76705.56 35.76 0.194 0.008 1.13-0.89 678 50 50 100.0 13.6 38608.48 14.42 0.154 0.020 0.88-0.76 543 49 49 100.0 11.1 33595.72 12.55 0.155 0.029 0.76-0.69 433 48 48 100.0 9.0 25005.54 9.87 0.152 0.031 0.69-0.63 380 54 51 94.4 7.5 18099.68 7.71 0.180 0.045 0.63-0.58 291 58 50 86.2 5.8 10167.21 4.51 0.208 0.053 0.58-0.55 199 56 49 87.5 4.1 16846.66 5.72 0.087 0.054 0.55-0.52 141 65 48 73.8 2.9 4040.68 2.26 0.108 0.117 0.52-0.49 117 82 48 58.5 2.4 12812.17 4.05 0.082 0.072 0.49-0.45 70 140 43 30.7 1.6 4393.57 1.50 0.417 0.886 -------------------------------------------------------------------------------------------- inf-0.45 3778 651 485 74.5 7.8 37543.97 15.95 0.174 0.026 inf-0.65 2817 227 224 98.7 12.6 45788.22 19.62 0.177 0.017 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.066387 0.013010 -0.008878 ( 0.000012 0.000013 0.000012 ) 0.014590 0.065201 -0.013162 ( 0.000011 0.000012 0.000011 ) 0.006107 -0.014641 -0.066252 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004657 -0.000002 -0.000007 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004635 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000007 -0.000004 0.004641 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.066387 0.013010 -0.008878 ( 0.000012 0.000013 0.000012 ) 0.014590 0.065201 -0.013162 ( 0.000011 0.000012 0.000011 ) 0.006107 -0.014641 -0.066252 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) unit cell: 10.3934(17) 10.419(2) 10.411(2) 89.955(16) 89.911(15) 89.977(15) V = 1127.4(4) unit cell: 10.4078(5) 10.4078(5) 10.4078(5) 90.0 90.0 90.0 V = 1127.40(9) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.175) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-565.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-588.7455 max=1111814.4646 PROFFIT INFO: background sum: min=-42.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=412.0000 max=5617.0000 PROFFIT INFO: num of signal pixels: min=41 max=497 PROFFIT INFO: Inet: min=-941.9929 max=1778903.2500 PROFFIT INFO: sig(Inet): min=57.5968 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.72 max=198.39 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 698 2702 4032 4812 5150 5984 6470 6776 7280 7578 7662 Percent 9.1 35.3 52.6 62.8 67.2 78.1 84.4 88.4 95.0 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3831 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 3831 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1778903- 126780 383 389443.27 76.08 100.00 126205- 3859 383 29071.80 19.45 100.00 3859- 2002 383 2774.99 6.85 97.13 1997- 1174 383 1534.09 3.83 50.39 1174- 788 383 967.44 2.22 11.75 786- 521 383 649.32 1.64 7.05 519- 317 383 411.65 1.19 4.70 316- 143 383 226.73 0.67 1.04 143- 10 383 73.84 0.27 0.00 10- -942 384 -132.06 -0.26 0.00 ------------------------------------------------------------------------------------ 1778903- -942 3831 42490.98 11.19 37.20 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 383 106187.90 14.91 67.10 1.64- 1.26 383 80993.82 21.81 59.79 1.26- 1.09 383 54901.24 17.87 65.01 1.09- 0.96 383 50802.87 14.17 34.20 0.96- 0.88 383 14450.43 6.52 40.47 0.88- 0.81 383 51644.51 14.51 36.81 0.81- 0.76 383 17858.00 5.63 17.49 0.76- 0.71 383 21480.42 7.01 17.75 0.71- 0.67 383 23333.76 7.82 27.94 0.67- 0.63 384 3359.00 1.71 5.47 ------------------------------------------------------------------------------------ 6.00- 0.63 3831 42490.98 11.19 37.20 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:39:39 2019 Sorting 3831 observations 43 unique observations with > 7.00 F2/sig(F2) 3831 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 74 382 Total number of frames 382 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 3831 observations in 4 runs Run # start # end # total # 1 0 11 12 2 0 11 24 3 0 11 36 4 0 8 45 Total number of frames 45 904 observations > 7.00 F2/sig(F2) 904 observations in 4 runs Run # start # end # total # 1 0 11 12 2 0 11 24 3 0 11 36 4 0 8 45 Total number of frames 45 Removing 'redundancy=1' reflections Average redundancy: 17.7 (Out of 904 removed 2 = 902, unique = 51) 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 902 observations in 4 runs Run # start # end # total # 1 0 11 12 2 0 11 24 3 0 11 36 4 0 8 45 Total number of frames 45 51 unique data precomputed (should be 51) 51 unique data with 902 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 17.7 (Out of 902 removed 0 = 902, unique = 51) 51 unique data precomputed (should be 51) 51 unique data with 902 observations RMS deviation of equivalent data = 0.28155 Rint = 0.20271 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19662, wR= 0.26628 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09127, wR= 0.14630, Acormin=0.577, Acormax=1.374, Acor_av=1.026 F test: Probability=1.000, F= 4.613 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08748, wR= 0.13728, Acormin=0.523, Acormax=1.453, Acor_av=0.991 F test: Probability=0.881, F= 1.085 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08191, wR= 0.14113, Acormin=0.588, Acormax=1.427, Acor_av=1.027 F test: Probability=0.999, F= 1.228 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08050, wR= 0.13027, Acormin=0.536, Acormax=1.541, Acor_av=0.998 F test: Probability=0.673, F= 1.031 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07489, wR= 0.12174, Acormin=0.571, Acormax=1.660, Acor_av=1.004 F test: Probability=0.992, F= 1.182 Final absorption model (ne=4, no=3): Rint= 0.07489, Acormin=0.571, Acormax=1.660, Acor_av=1.004 Combined refinement in use Rint: 0.20484 There are 45 active scales (one needs to be fixed) Refinement control: frame scale #21 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 68 pars with 2346 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.28155 Using Levenberg-Marquardt: 0.00010 New wR= 0.13372 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20271 with corrections 0.09433 Rint for all data: 0.20484 with corrections 0.09704 1 observations identified as outliers and rejected Cycle 2 wR= 0.12816 Using Levenberg-Marquardt: 0.00001 New wR= 0.11882 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20308 with corrections 0.07851 Rint for all data: 0.20484 with corrections 0.08496 2 observations identified as outliers and rejected Cycle 3 wR= 0.09919 Using Levenberg-Marquardt: 0.00000 New wR= 0.08871 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19892 with corrections 0.06025 Rint for all data: 0.20484 with corrections 0.06987 1 observations identified as outliers and rejected Cycle 4 wR= 0.08071 Using Levenberg-Marquardt: 0.00000 New wR= 0.08042 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19776 with corrections 0.05442 Rint for all data: 0.20484 with corrections 0.06551 1 observations identified as outliers and rejected Cycle 5 wR= 0.07577 Using Levenberg-Marquardt: 0.00000 New wR= 0.07638 Using Levenberg-Marquardt: 0.00000 New wR= 0.07638 Using Levenberg-Marquardt: 0.00000 New wR= 0.07638 Using Levenberg-Marquardt: 0.00001 New wR= 0.07638 Using Levenberg-Marquardt: 0.00010 New wR= 0.07638 Using Levenberg-Marquardt: 0.00100 New wR= 0.07637 Using Levenberg-Marquardt: 0.01000 New wR= 0.07632 Using Levenberg-Marquardt: 0.10000 New wR= 0.07608 Using Levenberg-Marquardt: 1.00000 New wR= 0.07581 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19719 with corrections 0.05320 Rint for all data: 0.20484 with corrections 0.06508 Final wR= 0.07581 Final frame scales: Min= 0.7998 Max= 1.2800 Final absorption correction factors: Amin= 0.5039 Amax= 1.3980 PROFFIT INFO: Inet (after scale3 abspack): min=-862.5034 max=1252981.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=46.1237 max=23015.0742 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/103 3831 reflections read from tmp file 164 reflections are rejected (163 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 1 5 7 2 6 3 3 129 Initial Chi^2= 0.51171 Cycle 1, Chi^2= 1.03428 Current error model SIG(F2)^2 = 68.34*I_RAW + 8.80*I_BACK+(0.03296*)^2 Cycle 2, Chi^2= 1.02243 Current error model SIG(F2)^2 = 82.63*I_RAW + 6.26*I_BACK+(0.02763*)^2 Cycle 3, Chi^2= 1.00367 Current error model SIG(F2)^2 = 85.89*I_RAW + 5.98*I_BACK+(0.02764*)^2 Cycle 4, Chi^2= 1.00061 Current error model SIG(F2)^2 = 86.44*I_RAW + 5.93*I_BACK+(0.02763*)^2 Cycle 5, Chi^2= 1.00010 Current error model SIG(F2)^2 = 86.52*I_RAW + 5.93*I_BACK+(0.02763*)^2 Final Chi^2= 1.00010 Final error model SIG(F2)^2 = 86.52*I_RAW + 5.93*I_BACK+(0.02763*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1252981- 116295 383 374694.06 29.80 100.00 116236- 3453 383 29269.42 12.77 100.00 3453- 1959 383 2642.99 5.95 99.22 1956- 1149 383 1490.01 3.90 67.10 1147- 753 383 923.22 2.65 20.89 753- 508 383 628.51 2.27 11.49 507- 310 383 402.81 1.91 9.14 309- 141 383 222.32 1.34 1.83 141- 10 383 73.74 0.67 0.00 10- -863 384 -128.34 -0.56 0.00 ------------------------------------------------------------------------------------ 1252981- -863 3831 41011.13 6.07 40.96 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 383 104712.00 9.80 69.97 1.64- 1.26 383 79260.73 9.22 62.92 1.26- 1.09 383 54412.08 7.85 69.71 1.09- 0.96 383 47629.56 6.39 37.08 0.96- 0.88 383 15300.39 4.58 48.30 0.88- 0.81 383 47369.19 7.46 42.30 0.81- 0.76 383 16754.00 3.66 19.58 0.76- 0.71 383 19493.28 4.82 20.89 0.71- 0.67 383 22069.98 5.26 32.11 0.67- 0.63 384 3208.84 1.64 6.77 ------------------------------------------------------------------------------------ 6.00- 0.63 3831 41011.13 6.07 40.96 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 383 104712.00 9.80 69.97 6.00- 1.26 766 91986.36 9.51 66.45 6.00- 1.09 1149 79461.60 8.96 67.54 6.00- 0.96 1532 71503.59 8.32 59.92 6.00- 0.88 1915 60262.95 7.57 57.60 6.00- 0.81 2298 58113.99 7.55 55.05 6.00- 0.76 2681 52205.42 7.00 49.98 6.00- 0.71 3064 48116.40 6.72 46.34 6.00- 0.67 3447 45222.36 6.56 44.76 6.00- 0.63 3831 41011.13 6.07 40.96 ------------------------------------------------------------------------------------ 6.00- 0.63 3831 41011.13 6.07 40.96 Scale applied to data: s=0.798096 (maximum obs:1252981.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.065; Rsigma 0.039: data 3831 -> merged 162 With outlier rejection... Rint 0.053; Rsigma 0.039: data 3816 -> merged 162 Rejected total: 15, method kkm 9, method Blessing 6 Completeness direct cell (a, b, c) = (10.408, 10.408, 10.408), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626476, 6.008949 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.76 14 14 24.93 100.00 349 1.73 - 1.27 14 14 27.64 100.00 387 1.26 - 1.06 14 14 31.07 100.00 435 1.05 - 0.97 14 14 26.93 100.00 377 0.95 - 0.88 14 14 28.21 100.00 395 0.87 - 0.81 14 14 24.93 100.00 349 0.80 - 0.76 14 14 26.57 100.00 372 0.76 - 0.72 14 14 21.86 100.00 306 0.72 - 0.69 14 14 24.00 100.00 336 0.69 - 0.65 19 19 20.32 100.00 386 --------------------------------------------------------------- 7.36 - 0.65 145 145 25.46 100.00 3692 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:39:39 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.373727 7.360010 7.370202 120.1791 120.0756 89.6258 3778 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.79 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1890 1891 1897 1882 2839 2516 2522 3778 N (int>3sigma) = 0 210 228 306 213 372 588 595 865 Mean intensity = 0.0 0.9 0.9 1.3 0.9 1.0 28.7 30.2 29.4 Mean int/sigma = 0.0 1.4 1.5 1.9 1.4 1.6 4.7 4.9 4.8 Lattice type: P chosen Volume: 282.66 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.360 7.364 119.78 90.18 119.84 Niggli form: a.a = 53.951 b.b = 54.170 c.c = 54.222 b.c = -26.915 a.c = -0.170 a.b = -26.901 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.297 CUBIC F-lattice R(int) = 0.237 [ 3541] Vol = 1130.6 Cell: 10.384 10.452 10.417 90.13 89.86 90.11 Volume: 1130.64 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.292 RHOMBOHEDRAL R-lattice R(int) = 0.219 [ 3106] Vol = 848.0 Cell: 7.360 7.345 18.084 89.84 90.30 119.84 Volume: 847.98 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.292 RHOMBOHEDRAL R-lattice R(int) = 0.228 [ 1005] Vol = 848.0 Trigonal Cell: 7.360 7.345 18.084 89.84 90.30 119.84 Volume: 847.98 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.496 TETRAGONAL I-lattice R(int) = 0.226 [ 3154] Vol = 565.3 Cell: 7.370 7.387 10.384 89.82 89.97 90.19 Volume: 565.32 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.491 TETRAGONAL I-lattice R(int) = 0.226 [ 3154] Vol = 565.3 Cell: 7.370 7.387 10.384 89.82 89.97 90.19 Volume: 565.32 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.378 ORTHORHOMBIC I-lattice R(int) = 0.191 [ 3081] Vol = 565.3 Cell: 7.370 10.384 7.387 89.82 89.81 90.03 Volume: 565.32 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.226 MONOCLINIC I-lattice R(int) = 0.187 [ 2565] Vol = 565.3 Cell: 10.384 7.370 7.387 90.19 90.18 90.03 Volume: 565.32 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.186 MONOCLINIC I-lattice R(int) = 0.161 [ 2553] Vol = 565.3 Cell: 7.364 7.345 10.452 90.01 90.17 89.82 Volume: 565.32 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.220 MONOCLINIC C-lattice R(int) = 0.173 [ 2578] Vol = 565.3 Cell: 10.384 10.452 7.345 90.01 134.84 90.11 Volume: 565.32 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) = 0.111 [ 1616] Vol = 282.7 Cell: 7.345 7.360 7.364 119.78 90.18 119.84 Volume: 282.66 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 1897 0 2522 2506 3778 N (int>3sigma) = 0 0 0 0 306 0 595 586 865 Mean intensity = 0.0 0.0 0.0 0.0 1.3 0.0 30.2 29.7 29.4 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.9 4.8 4.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.978 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 26 26 285 724 N I>3s 0 0 0 180 0.0 0.0 -0.0 1.8 0.5 0.5 0.1 2.5 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 0.237 3284 Fd-3m 1 1 227 C N N N N 37 2284 0.236 3348 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.384253 10.452295 10.416986 90.1275 89.8568 90.1067 ZERR 1.00 0.005959 0.000998 0.010789 0.0997 0.0031 0.0049 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1126240- 95087 468 459 27 17.0 325542.91 28.03 0.049 0.063 74430- 1742 721 717 27 26.6 5180.85 8.08 0.095 0.112 1642- 763 752 751 27 27.8 1116.76 2.93 0.234 0.302 680- 345 727 727 27 26.9 493.11 1.91 0.390 0.550 324- 65 586 586 27 21.7 220.36 1.17 0.582 0.891 60- -154 577 576 27 21.3 5.56 0.17 0.967 3.853 ------------------------------------------------------------------------------------------- 1126240- -154 3831 3816 162 23.6 40479.13 6.04 0.053 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-1.27 739 734 27 27.2 93208.09 9.72 0.045 0.057 0.031 1.26-0.97 815 812 28 29.0 47721.98 6.74 0.049 0.064 0.035 0.95-0.81 746 744 28 26.6 32190.78 6.16 0.056 0.076 0.044 0.80-0.73 660 659 27 24.4 17137.59 4.05 0.072 0.092 0.056 0.72-0.67 583 581 27 21.5 18853.21 4.59 0.087 0.114 0.063 0.66-0.63 288 286 25 11.4 3867.33 1.77 0.115 0.073 0.127 ------------------------------------------------------------------------------------------------------ inf-0.63 3831 3816 162 23.6 40479.13 6.04 0.053 0.067 0.039 inf-0.65 3703 3690 144 25.6 41637.11 6.17 0.053 0.066 0.038 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-1.27 734 27 27 100.0 27.2 93208.09 48.96 0.045 0.008 1.26-0.97 812 28 28 100.0 29.0 47721.98 34.47 0.049 0.008 0.95-0.81 744 28 28 100.0 26.6 32190.78 32.48 0.056 0.011 0.80-0.73 659 27 27 100.0 24.4 17137.59 18.34 0.072 0.014 0.72-0.67 581 27 27 100.0 21.5 18853.21 23.38 0.087 0.014 0.66-0.63 286 25 25 100.0 11.4 3867.33 6.38 0.115 0.041 -------------------------------------------------------------------------------------------- inf-0.63 3816 162 162 100.0 23.6 40479.13 30.29 0.053 0.011 inf-0.65 3690 144 144 100.0 25.6 41637.11 31.14 0.053 0.010 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:46:18 2019) ID: 3668; threads 40; handles 809; mem 515356.00 (1204688.00)kB; time: 1w 4d 23h 57m 6s MEMORY INFO: Memory PF:279.0, Ph:624.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:503.3,peak PF: 700.2, WS: 471.3, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:281.0, Ph:626.0, V:1178.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:505.1,peak PF: 700.2, WS: 473.1, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:46:18 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000088 0.000065 0.000089 ) 0.064809 0.092374 0.027273 ( 0.000107 0.000079 0.000108 ) 0.045523 0.057900 0.132205 ( 0.000128 0.000095 0.000130 ) 7.38096 ( 0.00687 ) 7.36649 ( 0.00748 ) 7.42630 ( 0.00866 ) 120.52449 ( 0.11617 ) 120.40327 ( 0.11143 ) 89.27095 ( 0.07882 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:46:18 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000088 0.000065 0.000089 ) 0.064809 0.092374 0.027273 ( 0.000107 0.000079 0.000108 ) 0.045523 0.057900 0.132205 ( 0.000128 0.000095 0.000130 ) M - matrix: 0.013755 0.004510 0.009146 ( 0.000024 0.000016 0.000021 ) 0.004510 0.013967 0.009331 ( 0.000016 0.000019 0.000018 ) 0.009146 0.009331 0.018528 ( 0.000021 0.000018 0.000035 ) unit cell: 7.381(7) 7.366(7) 7.426(9) 120.52(12) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.82 | 24 | 1.005 ( 0.047) | 1.008 ( 0.130) | 0.907 ( 0.354) | 0.79- 0.69 | 24 | 0.998 ( 0.044) | 1.006 ( 0.137) | 1.289 ( 0.497) | 0.69- 0.63 | 23 | 0.979 ( 0.051) | 0.913 ( 0.103) | 1.157 ( 0.432) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.510) | 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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb PROFFITPEAK info: 402 peaks in the peak location table UB fit with 45 obs out of 226 (total:226,skipped:0) (19.91%) UB - matrix: 0.086386 -0.045965 0.017145 ( 0.000486 0.000166 0.000234 ) 0.064465 0.092962 0.027826 ( 0.000643 0.000220 0.000310 ) 0.045451 0.058297 0.132814 ( 0.000847 0.000290 0.000408 ) M - matrix: 0.013684 0.004672 0.009311 ( 0.000141 0.000084 0.000119 ) 0.004672 0.014153 0.009541 ( 0.000084 0.000055 0.000055 ) 0.009311 0.009541 0.018708 ( 0.000119 0.000055 0.000110 ) unit cell: 7.46(3) 7.36(3) 7.42(3) 120.7(5) 120.3(5) 89.5(4) V = 285(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 4, #refl in peak table: 226 #indexed refl 206, indexation with best UB: 91.1504% Lattice: 7.4033 7.3552 7.3602 119.996 120.271 89.814 282.712 Rotation: -22.654 24.751 -35.031 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 217 obs out of 226 (total:226,skipped:0) (96.02%) UB - matrix: 0.087754 -0.044390 0.012610 ( 0.000056 0.000058 0.000062 ) 0.061484 0.094372 0.026211 ( 0.000065 0.000067 0.000071 ) 0.049413 0.055449 0.133225 ( 0.000061 0.000064 0.000068 ) M - matrix: 0.013923 0.004647 0.009301 ( 0.000014 0.000010 0.000011 ) 0.004647 0.013951 0.009301 ( 0.000010 0.000015 0.000012 ) 0.009301 0.009301 0.018595 ( 0.000011 0.000012 0.000018 ) unit cell: 7.367(5) 7.356(5) 7.361(5) 120.01(7) 120.06(7) 89.97(5) V = 281.9(3) OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 UB - matrix: 0.087828 -0.044342 0.012557 ( 0.000055 0.000058 0.000061 ) 0.061529 0.094418 0.026188 ( 0.000063 0.000067 0.000071 ) 0.049447 0.055473 0.133193 ( 0.000058 0.000061 0.000065 ) M - matrix: 0.013945 0.004658 0.009300 ( 0.000014 0.000010 0.000011 ) 0.004658 0.013958 0.009304 ( 0.000010 0.000015 0.000012 ) 0.009300 0.009304 0.018584 ( 0.000011 0.000012 0.000018 ) UB fit with 219 obs out of 226 (total:226,skipped:0) (96.90%) unit cell: 7.359(5) 7.355(5) 7.361(5) 120.01(7) 120.01(7) 90.01(5) V = 281.6(3) UB fit with 219 obs out of 226 (total:226,skipped:0) (96.90%) UB - matrix: 0.087828 -0.044342 0.012557 ( 0.000055 0.000058 0.000061 ) 0.061529 0.094418 0.026188 ( 0.000063 0.000067 0.000071 ) 0.049447 0.055473 0.133193 ( 0.000058 0.000061 0.000065 ) M - matrix: 0.013945 0.004658 0.009300 ( 0.000014 0.000010 0.000011 ) 0.004658 0.013958 0.009304 ( 0.000010 0.000015 0.000012 ) 0.009300 0.009304 0.018584 ( 0.000011 0.000012 0.000018 ) unit cell: 7.359(5) 7.355(5) 7.361(5) 120.01(7) 120.01(7) 90.01(5) V = 281.6(3) OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 UB - matrix: 0.087828 -0.044342 0.012557 ( 0.000055 0.000058 0.000061 ) 0.061529 0.094418 0.026188 ( 0.000063 0.000067 0.000071 ) 0.049447 0.055473 0.133193 ( 0.000058 0.000061 0.000065 ) M - matrix: 0.013945 0.004658 0.009300 ( 0.000014 0.000010 0.000011 ) 0.004658 0.013958 0.009304 ( 0.000010 0.000015 0.000012 ) 0.009300 0.009304 0.018584 ( 0.000011 0.000012 0.000018 ) UB fit with 219 obs out of 226 (total:226,skipped:0) (96.90%) unit cell: 7.359(5) 7.355(5) 7.361(5) 120.01(7) 120.01(7) 90.01(5) V = 281.6(3) 226 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Run 4 Omega scan: (-6.000 - 94.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1277 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087828 -0.044342 0.012557 ( 0.000055 0.000058 0.000061 ) 0.061529 0.094418 0.026188 ( 0.000063 0.000067 0.000071 ) 0.049447 0.055473 0.133193 ( 0.000058 0.000061 0.000065 ) M - matrix: 0.013945 0.004658 0.009300 ( 0.000014 0.000010 0.000011 ) 0.004658 0.013958 0.009304 ( 0.000010 0.000015 0.000012 ) 0.009300 0.009304 0.018584 ( 0.000011 0.000012 0.000018 ) UB fit with 219 obs out of 226 (total:226,skipped:0) (96.90%) unit cell: 7.359(5) 7.355(5) 7.361(5) 120.01(7) 120.01(7) 90.01(5) V = 281.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 219 obs out of 226 (total:226,skipped:0) (96.90%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.95- 2.39 | 21 | 0.881 ( 0.096) | 0.886 ( 0.134) | 0.897 ( 0.398) | 2.38- 1.83 | 21 | 0.894 ( 0.111) | 0.918 ( 0.158) | 0.932 ( 0.282) | 1.76- 1.57 | 21 | 0.876 ( 0.117) | 0.895 ( 0.167) | 0.786 ( 0.271) | 1.57- 1.35 | 21 | 0.953 ( 0.086) | 0.984 ( 0.133) | 0.796 ( 0.401) | 1.35- 1.19 | 21 | 0.944 ( 0.077) | 0.955 ( 0.102) | 1.006 ( 0.479) | 1.19- 1.00 | 21 | 0.957 ( 0.087) | 0.973 ( 0.119) | 0.881 ( 0.305) | 1.00- 0.88 | 21 | 0.991 ( 0.066) | 1.005 ( 0.081) | 1.059 ( 0.405) | 0.88- 0.79 | 21 | 0.996 ( 0.044) | 1.000 ( 0.120) | 0.980 ( 0.320) | 0.79- 0.69 | 21 | 0.973 ( 0.045) | 0.930 ( 0.088) | 1.188 ( 0.475) | 0.69- 0.63 | 23 | 0.929 ( 0.046) | 0.853 ( 0.071) | 1.259 ( 0.441) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.95- 0.63 | 212 | 0.939 ( 0.091) | 0.939 ( 0.131) | 0.981 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 212 obs out of 212 (total:212,skipped:0) (100.00%) UB - matrix: 0.088073 -0.044303 0.012812 ( 0.000028 0.000031 0.000032 ) 0.061423 0.094491 0.026073 ( 0.000022 0.000025 0.000026 ) 0.049325 0.055390 0.133176 ( 0.000021 0.000024 0.000024 ) M - matrix: 0.013963 0.004634 0.009299 ( 0.000006 0.000004 0.000005 ) 0.004634 0.013959 0.009273 ( 0.000004 0.000006 0.000005 ) 0.009299 0.009273 0.018580 ( 0.000005 0.000005 0.000007 ) unit cell: 7.352(2) 7.343(2) 7.3528(18) 119.92(3) 120.05(3) 89.96(2) V = 280.90(13) OTKP changes: 212 1 1 1 OTKP changes: 212 1 1 1 OTKP changes: 212 1 1 1 UB - matrix: 0.087887 -0.044360 0.012685 ( 0.000022 0.000025 0.000026 ) 0.061498 0.094412 0.026180 ( 0.000021 0.000024 0.000025 ) 0.049388 0.055444 0.133227 ( 0.000020 0.000022 0.000023 ) M - matrix: 0.013945 0.004646 0.009305 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013955 0.009296 ( 0.000004 0.000006 0.000004 ) 0.009305 0.009296 0.018596 ( 0.000004 0.000004 0.000006 ) UB fit with 212 obs out of 212 (total:212,skipped:0) (100.00%) unit cell: 7.3592(18) 7.3516(19) 7.3577(17) 119.98(2) 120.05(2) 89.97(2) V = 281.41(12) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 94.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087887 -0.044360 0.012685 ( 0.000022 0.000025 0.000026 ) 0.061498 0.094412 0.026180 ( 0.000021 0.000024 0.000025 ) 0.049388 0.055444 0.133227 ( 0.000020 0.000022 0.000023 ) M - matrix: 0.013945 0.004646 0.009305 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013955 0.009296 ( 0.000004 0.000006 0.000004 ) 0.009305 0.009296 0.018596 ( 0.000004 0.000004 0.000006 ) UB fit with 212 obs out of 212 (total:212,skipped:0) (100.00%) unit cell: 7.3592(18) 7.3516(19) 7.3577(17) 119.98(2) 120.05(2) 89.97(2) V = 281.41(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 212 obs out of 212 (total:212,skipped:0) (100.00%) 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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb 0 of 211 peaks identified as outliers and rejected 211 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 211 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 211 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 21 | 0.875 ( 0.100) | 0.887 ( 0.126) | 0.886 ( 0.391) | 2.38- 1.83 | 21 | 0.892 ( 0.112) | 0.909 ( 0.165) | 0.947 ( 0.286) | 1.76- 1.58 | 21 | 0.878 ( 0.117) | 0.903 ( 0.169) | 0.745 ( 0.279) | 1.57- 1.35 | 21 | 0.955 ( 0.084) | 0.980 ( 0.131) | 0.838 ( 0.449) | 1.35- 1.19 | 21 | 0.939 ( 0.078) | 0.953 ( 0.093) | 0.940 ( 0.502) | 1.19- 1.00 | 21 | 0.971 ( 0.082) | 0.991 ( 0.120) | 0.863 ( 0.280) | 1.00- 0.88 | 21 | 0.988 ( 0.066) | 1.012 ( 0.075) | 1.033 ( 0.361) | 0.88- 0.79 | 21 | 0.992 ( 0.043) | 0.995 ( 0.119) | 1.026 ( 0.377) | 0.79- 0.69 | 21 | 0.970 ( 0.044) | 0.928 ( 0.090) | 1.254 ( 0.484) | 0.69- 0.63 | 22 | 0.928 ( 0.049) | 0.850 ( 0.075) | 1.257 ( 0.451) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 211 | 0.939 ( 0.092) | 0.940 ( 0.131) | 0.980 ( 0.426) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 92 | 0.982 ( 0.036) | 1.030 ( 0.070) | 1.117 ( 0.492) | 10.4-14.9 | 92 | 0.983 ( 0.044) | 1.040 ( 0.070) | 1.169 ( 0.546) | 14.9-19.0 | 92 | 0.994 ( 0.220) | 1.020 ( 0.097) | 1.206 ( 1.139) | 19.0-23.6 | 92 | 0.957 ( 0.055) | 0.999 ( 0.080) | 0.934 ( 0.421) | 23.6-27.4 | 92 | 0.959 ( 0.064) | 0.992 ( 0.094) | 0.938 ( 0.423) | 27.5-32.6 | 92 | 0.946 ( 0.084) | 0.959 ( 0.114) | 0.926 ( 0.444) | 32.6-36.4 | 92 | 0.919 ( 0.163) | 0.899 ( 0.133) | 1.092 ( 0.652) | 36.4-39.0 | 92 | 0.877 ( 0.092) | 0.845 ( 0.124) | 1.014 ( 0.501) | 39.0-42.0 | 92 | 0.893 ( 0.095) | 0.837 ( 0.123) | 1.065 ( 0.486) | 42.0-50.1 | 88 | 0.873 ( 0.118) | 0.796 ( 0.136) | 0.941 ( 0.451) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 916 | 0.938 ( 0.119) | 0.942 ( 0.136) | 1.041 ( 0.601) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.13 e2 dimension: a=-0.0071 b=1.25 e3 dimension: a=0.0011 b=1.07 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3814 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:46:32 2019 PROFFITMAIN - Started at Wed Aug 21 13:46:32 2019 OTKP changes: 347 2 3 4 OTKP changes: 347 2 3 4 OTKP changes: 347 2 3 4 UB - matrix: 0.087697 -0.045999 0.016738 ( 0.000083 0.000065 0.000084 ) 0.063178 0.092380 0.026747 ( 0.000093 0.000073 0.000095 ) 0.045315 0.057604 0.131888 ( 0.000096 0.000075 0.000097 ) M - matrix: 0.013736 0.004413 0.009134 ( 0.000021 0.000014 0.000017 ) 0.004413 0.013968 0.009298 ( 0.000014 0.000017 0.000015 ) 0.009134 0.009298 0.018390 ( 0.000017 0.000015 0.000026 ) UB fit with 399 obs out of 916 (total:916,skipped:0) (43.56%) unit cell: 7.397(6) 7.370(7) 7.440(7) 120.79(10) 120.33(9) 88.72(7) V = 285.1(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 201 obs out of 212 (total:212,skipped:0) (94.81%) UB - matrix: 0.087614 -0.046166 0.017183 ( 0.000107 0.000066 0.000100 ) 0.064570 0.092364 0.027087 ( 0.000092 0.000057 0.000086 ) 0.045797 0.057738 0.132020 ( 0.000109 0.000067 0.000102 ) M - matrix: 0.013943 0.004563 0.009301 ( 0.000024 0.000014 0.000019 ) 0.004563 0.013996 0.009331 ( 0.000014 0.000014 0.000014 ) 0.009301 0.009331 0.018458 ( 0.000019 0.000014 0.000028 ) unit cell: 7.373(7) 7.364(7) 7.439(7) 120.53(10) 120.46(10) 89.14(7) V = 283.4(4) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.179) HKL list info: 1285 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087481 -0.046176 0.017355 ( 0.000100 0.000062 0.000093 ) 0.064777 0.092356 0.027259 ( 0.000086 0.000053 0.000080 ) 0.045687 0.057804 0.132107 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013936 0.004584 0.009320 ( 0.000023 0.000013 0.000018 ) 0.004584 0.014003 0.009353 ( 0.000013 0.000014 0.000013 ) 0.009320 0.009353 0.018497 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.379(6) 7.366(6) 7.435(6) 120.52(9) 120.47(9) 89.21(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 204 obs out of 212 (total:212,skipped:0) (96.23%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.117974 0.038991 0.078615 ( 0.000076 0.000047 0.000070 ) 0.000083 0.111530 0.056276 ( 0.000080 0.000050 0.000074 ) -0.000027 -0.000078 0.095357 ( 0.000089 0.000056 0.000083 ) M - matrix: 0.013918 0.004609 0.009277 ( 0.000018 0.000011 0.000014 ) 0.004609 0.013959 0.009334 ( 0.000011 0.000012 0.000011 ) 0.009277 0.009334 0.018440 ( 0.000014 0.000011 0.000021 ) UB fit with 207 obs out of 212 (total:212,skipped:0) (97.64%) unit cell: 7.375(5) 7.382(5) 7.434(8) 120.48(9) 120.25(9) 89.46(6) V = 284.3(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.087804 -0.044309 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094149 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055798 0.133161 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004658 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009312 0.018585 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3551(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) UB - matrix: 0.087894 -0.044371 0.012683 ( 0.000023 0.000025 0.000027 ) 0.061490 0.094409 0.026168 ( 0.000021 0.000023 0.000024 ) 0.049392 0.055431 0.133222 ( 0.000019 0.000021 0.000022 ) M - matrix: 0.013946 0.004643 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013954 0.009292 ( 0.000004 0.000006 0.000004 ) 0.009304 0.009292 0.018594 ( 0.000004 0.000004 0.000006 ) unit cell: 7.3589(18) 7.3509(19) 7.3574(16) 119.98(2) 120.06(2) 89.96(2) V = 281.39(12) OTKP changes: 211 1 1 1 OTKP changes: 211 1 1 1 OTKP changes: 211 1 1 1 OTKP changes: 211 1 1 1 OTKP changes: 211 1 1 1 OTKP changes: 211 1 1 1 Run 4 Omega scan: (-6.000 - 94.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1255 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087894 -0.044371 0.012683 ( 0.000023 0.000025 0.000027 ) 0.061490 0.094409 0.026168 ( 0.000021 0.000023 0.000024 ) 0.049392 0.055431 0.133222 ( 0.000019 0.000021 0.000022 ) M - matrix: 0.013946 0.004643 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013954 0.009292 ( 0.000004 0.000006 0.000004 ) 0.009304 0.009292 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) unit cell: 7.3589(18) 7.3509(19) 7.3574(16) 119.98(2) 120.06(2) 89.96(2) V = 281.39(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* UB - matrix: 0.118100 0.039334 0.078780 ( 0.000023 0.000026 0.000027 ) 0.000003 0.111387 0.055610 ( 0.000011 0.000013 0.000013 ) -0.000004 0.000000 0.096408 ( 0.000025 0.000029 0.000030 ) M - matrix: 0.013948 0.004646 0.009304 ( 0.000005 0.000003 0.000004 ) 0.004646 0.013954 0.009293 ( 0.000003 0.000004 0.000004 ) 0.009304 0.009293 0.018593 ( 0.000004 0.000004 0.000007 ) UB fit with 211 obs out of 211 (total:211,skipped:0) (100.00%) unit cell: 7.3582(18) 7.3513(14) 7.357(3) 119.98(3) 120.05(3) 89.973(18) V = 281.37(12) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 68.89 ph= 0.28 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\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117641 0.038634 0.078478 ( 0.000040 0.000039 0.000044 ) -0.000001 0.111478 0.056062 ( 0.000026 0.000025 0.000029 ) -0.000051 -0.000131 0.096142 ( 0.000029 0.000027 0.000031 ) M - matrix: 0.013839 0.004545 0.009227 ( 0.000009 0.000006 0.000007 ) 0.004545 0.013920 0.009269 ( 0.000006 0.000006 0.000006 ) 0.009227 0.009269 0.018545 ( 0.000007 0.000006 0.000010 ) UB fit with 909 obs out of 916 (total:916,skipped:0) (99.24%) unit cell: 7.376(3) 7.360(2) 7.371(3) 120.18(3) 120.10(4) 89.59(3) V = 282.76(16) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 88 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof 4080 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:46:38 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.179) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 94.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-565.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-588.7455 max=1113635.6190 PROFFIT INFO: background sum: min=-50.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=396.0000 max=5594.0000 PROFFIT INFO: num of signal pixels: min=41 max=498 PROFFIT INFO: Inet: min=-941.9929 max=1781817.0000 PROFFIT INFO: sig(Inet): min=57.6010 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.72 max=198.42 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 364 1443 2144 2560 2746 3184 3445 3611 3877 4037 4080 Percent 8.9 35.4 52.5 62.7 67.3 78.0 84.4 88.5 95.0 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4080 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 4080 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1781817- 124037 408 389526.79 75.52 100.00 123971- 3845 408 28760.36 19.34 100.00 3836- 1999 408 2761.97 6.91 97.30 1996- 1165 408 1526.10 3.77 48.77 1164- 792 408 964.42 2.21 12.01 790- 518 408 648.14 1.69 8.33 518- 320 408 413.07 1.17 5.15 320- 144 408 230.59 0.68 0.98 144- 13 408 75.19 0.27 0.00 13- -942 408 -135.79 -0.27 0.00 ------------------------------------------------------------------------------------ 1781817- -942 4080 42477.08 11.13 37.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 408 93831.42 15.89 69.36 1.75- 1.26 408 93672.11 21.64 58.33 1.26- 1.04 408 56850.74 16.67 52.70 1.04- 0.90 408 33789.20 10.29 37.75 0.90- 0.81 408 26560.30 8.74 32.11 0.81- 0.74 408 36818.53 11.11 37.75 0.74- 0.68 408 26207.99 8.28 25.49 0.68- 0.62 408 23018.89 7.24 23.28 0.62- 0.56 408 19688.09 6.51 20.34 0.56- 0.44 408 14333.57 4.94 15.44 ------------------------------------------------------------------------------------ 6.55- 0.44 4080 42477.08 11.13 37.25 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:46:38 2019 Sorting 4080 observations 87 unique observations with > 7.00 F2/sig(F2) 4080 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 99 407 Total number of frames 407 Maximum number of 87 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 4080 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 19 83 Total number of frames 83 967 observations > 7.00 F2/sig(F2) 967 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 19 83 Total number of frames 83 Removing 'redundancy=1' reflections Average redundancy: 7.5 (Out of 967 removed 32 = 935, unique = 125) 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 935 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 19 83 Total number of frames 83 125 unique data precomputed (should be 125) 125 unique data with 935 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.5 (Out of 935 removed 0 = 935, unique = 125) 125 unique data precomputed (should be 125) 125 unique data with 935 observations RMS deviation of equivalent data = 0.39313 Rint = 0.35129 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.35060, wR= 0.47874 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26143, wR= 0.35879, Acormin=0.515, Acormax=1.463, Acor_av=1.026 F test: Probability=1.000, F= 1.787 Trying model 2 (ne=2, no=1)... Results: Rint= 0.25265, wR= 0.35395, Acormin=0.526, Acormax=1.489, Acor_av=0.989 F test: Probability=0.820, F= 1.067 Trying model 3 (ne=4, no=0)... Results: Rint= 0.25549, wR= 0.34892, Acormin=0.496, Acormax=1.625, Acor_av=0.978 F test: Probability=0.688, F= 1.035 Trying model 4 (ne=4, no=1)... Results: Rint= 0.23994, wR= 0.33934, Acormin=0.387, Acormax=1.672, Acor_av=0.956 F test: Probability=0.986, F= 1.169 Trying model 5 (ne=4, no=3)... Results: Rint= 0.23766, wR= 0.32592, Acormin=0.273, Acormax=1.774, Acor_av=0.873 F test: Probability=0.557, F= 1.010 Trying model 6 (ne=6, no=0)... Results: Rint= 0.25508, wR= 0.33336, Acormin=0.240, Acormax=1.606, Acor_av=0.929 F test: Probability=0.000, F= 0.874 Trying model 7 (ne=6, no=1)... Results: Rint= 0.23922, wR= 0.31992, Acormin=0.211, Acormax=1.671, Acor_av=0.933 F test: Probability=0.000, F= 0.990 Trying model 8 (ne=6, no=3)... Results: Rint= 0.24420, wR= 0.31510, Acormin=0.162, Acormax=1.823, Acor_av=0.826 F test: Probability=0.000, F= 0.941 Trying model 9 (ne=6, no=5)... Results: Rint= 0.25030, wR= 0.32397, Acormin=0.182, Acormax=2.001, Acor_av=0.754 F test: Probability=0.000, F= 0.883 Trying model 10 (ne=8, no=0)... Results: Rint= 0.26966, wR= 0.32724, Acormin=-0.034, Acormax=1.629, Acor_av=0.830 F test: Probability=0.000, F= 0.765 Trying model 11 (ne=8, no=1)... Results: Rint= 0.31899, wR= 0.36838, Acormin=-0.006, Acormax=1.314, Acor_av=0.613 F test: Probability=0.000, F= 0.544 Trying model 12 (ne=8, no=3)... Results: Rint= 0.32470, wR= 0.37564, Acormin=-0.004, Acormax=0.108, Acor_av=0.039 F test: Probability=0.000, F= 0.521 Trying model 13 (ne=8, no=5)... Results: Rint= 0.29774, wR= 0.35119, Acormin=-0.002, Acormax=0.112, Acor_av=0.042 F test: Probability=0.000, F= 0.610 Trying model 14 (ne=8, no=7)... Results: Rint= 0.23857, wR= 0.30332, Acormin=-0.007, Acormax=0.157, Acor_av=0.044 F test: Probability=0.000, F= 0.931 Final absorption model (ne=4, no=1): Rint= 0.23994, Acormin=0.387, Acormax=1.672, Acor_av=0.956 Combined refinement in use Rint: 0.36546 There are 83 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 1 (17 parameters) Refinement control: 99 pars with 4950 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.39313 Using Levenberg-Marquardt: 0.00010 New wR= 0.22635 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35129 with corrections 0.19366 Rint for all data: 0.36546 with corrections 0.20953 0 observations identified as outliers and rejected Cycle 2 wR= 0.22635 Using Levenberg-Marquardt: 0.00001 New wR= 0.21668 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35129 with corrections 0.18512 Rint for all data: 0.36546 with corrections 0.20106 0 observations identified as outliers and rejected Cycle 3 wR= 0.21668 Using Levenberg-Marquardt: 0.00000 New wR= 0.21592 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35129 with corrections 0.18383 Rint for all data: 0.36546 with corrections 0.19979 0 observations identified as outliers and rejected Cycle 4 wR= 0.21592 Using Levenberg-Marquardt: 0.00000 New wR= 0.21682 Using Levenberg-Marquardt: 0.00000 New wR= 0.21682 Using Levenberg-Marquardt: 0.00001 New wR= 0.21682 Using Levenberg-Marquardt: 0.00010 New wR= 0.21680 Using Levenberg-Marquardt: 0.00100 New wR= 0.21663 Using Levenberg-Marquardt: 0.01000 New wR= 0.21557 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35129 with corrections 0.18284 Rint for all data: 0.36546 with corrections 0.19885 0 observations identified as outliers and rejected Cycle 5 wR= 0.21557 Using Levenberg-Marquardt: 0.00100 New wR= 0.21808 Using Levenberg-Marquardt: 0.01000 New wR= 0.21676 Using Levenberg-Marquardt: 0.10000 New wR= 0.21509 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35129 with corrections 0.18273 Rint for all data: 0.36546 with corrections 0.19878 0 observations identified as outliers and rejected Final wR= 0.21509 Final frame scales: Min= 0.7926 Max= 4.1565 Final absorption correction factors: Amin= 0.3295 Amax= 1.7207 PROFFIT INFO: Inet (after scale3 abspack): min=-1592.0115 max=1798823.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=40.5373 max=38814.4141 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/103 4080 reflections read from tmp file 1016 reflections are rejected (958 as outliers, 58 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 77 44 38 35 39 27 22 21 122 Initial Chi^2= 2.21591 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.87048 Current error model SIG(F2)^2 = 477.49*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 415.64*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 415.64*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1798823- 109414 408 348916.23 31.45 100.00 108036- 3755 408 24743.01 6.72 81.37 3728- 1870 408 2488.82 2.61 27.94 1867- 1112 408 1460.48 1.97 16.67 1110- 697 408 883.01 1.33 1.23 697- 464 408 574.46 1.13 0.25 464- 279 408 363.32 1.00 0.98 279- 130 408 204.84 0.83 0.00 130- 11 408 67.38 0.47 0.25 11- -1592 408 -157.25 -0.34 0.00 ------------------------------------------------------------------------------------ 1798823- -1592 4080 37954.43 4.72 22.87 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 408 87550.23 10.67 52.70 1.75- 1.26 408 88235.66 9.19 39.22 1.26- 1.04 408 54600.61 6.29 33.82 1.04- 0.90 408 30364.52 3.74 15.69 0.90- 0.81 408 22948.10 3.25 13.73 0.81- 0.74 408 32967.12 3.94 20.10 0.74- 0.68 408 21722.88 3.03 13.97 0.68- 0.62 408 17862.73 2.68 13.24 0.62- 0.56 408 14329.92 2.44 14.95 0.56- 0.44 408 8962.55 1.93 11.27 ------------------------------------------------------------------------------------ 6.55- 0.44 4080 37954.43 4.72 22.87 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 408 87550.23 10.67 52.70 6.55- 1.26 816 87892.94 9.93 45.96 6.55- 1.04 1224 76795.50 8.72 41.91 6.55- 0.90 1632 65187.75 7.48 35.36 6.55- 0.81 2040 56739.82 6.63 31.03 6.55- 0.74 2448 52777.70 6.18 29.21 6.55- 0.68 2856 48341.30 5.73 27.03 6.55- 0.62 3264 44531.48 5.35 25.31 6.55- 0.56 3672 41175.75 5.03 24.16 6.55- 0.44 4080 37954.43 4.72 22.87 ------------------------------------------------------------------------------------ 6.55- 0.44 4080 37954.43 4.72 22.87 Scale applied to data: s=0.555918 (maximum obs:1798823.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.199; Rsigma 0.051: data 4080 -> merged 486 With outlier rejection... Rint 0.177; Rsigma 0.052: data 4009 -> merged 486 Rejected total: 71, method kkm 49, method Blessing 22 Completeness direct cell (a, b, c) = (6.564, 6.564, 6.564), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445561, 6.563527 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.59 22 22 21.32 100.00 469 1.55 - 1.22 22 22 19.05 100.00 419 1.20 - 1.03 22 22 16.86 100.00 371 1.03 - 0.92 22 22 13.73 100.00 302 0.92 - 0.84 22 22 14.00 100.00 308 0.84 - 0.79 22 22 11.23 100.00 247 0.79 - 0.75 22 22 11.64 100.00 256 0.75 - 0.71 22 22 9.14 100.00 201 0.71 - 0.69 22 22 9.45 100.00 208 0.68 - 0.65 27 29 8.85 93.10 239 --------------------------------------------------------------- 7.36 - 0.65 225 227 13.42 99.12 3020 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:46:39 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.375815 7.360342 7.370613 120.1801 120.1007 89.5854 4009 Reflections read from file xs2212a.hkl 4009 Reflections used for space-group determination (up to diffraction limit of 0.46A); mean (I/sigma) = 4.59 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2007 2009 2026 2011 3021 2663 2674 4009 N (int>3sigma) = 0 218 237 321 219 388 606 614 897 Mean intensity = 0.0 0.6 0.7 0.9 0.6 0.7 19.8 20.9 20.2 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.5 4.7 4.6 Lattice type: P chosen Volume: 282.76 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.360 7.362 119.74 90.19 119.84 Niggli form: a.a = 53.955 b.b = 54.175 c.c = 54.199 b.c = -26.880 a.c = -0.181 a.b = -26.902 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.319 CUBIC F-lattice R(int) = 0.249 [ 3771] Vol = 1131.0 Cell: 10.382 10.458 10.417 90.15 89.87 90.12 Volume: 1131.03 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.318 RHOMBOHEDRAL R-lattice R(int) = 0.225 [ 3337] Vol = 848.3 Cell: 7.360 7.345 18.088 89.83 90.35 119.84 Volume: 848.27 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.318 RHOMBOHEDRAL R-lattice R(int) = 0.226 [ 1078] Vol = 848.3 Trigonal Cell: 7.360 7.345 18.088 89.83 90.35 119.84 Volume: 848.27 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.529 TETRAGONAL I-lattice R(int) = 0.227 [ 3383] Vol = 565.5 Cell: 7.371 7.390 10.382 89.82 89.99 90.22 Volume: 565.51 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.520 TETRAGONAL I-lattice R(int) = 0.227 [ 3383] Vol = 565.5 Cell: 7.371 7.390 10.382 89.82 89.99 90.22 Volume: 565.51 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.364 ORTHORHOMBIC I-lattice R(int) = 0.186 [ 3312] Vol = 565.5 Cell: 7.371 10.382 7.390 89.82 89.78 90.01 Volume: 565.51 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.231 MONOCLINIC I-lattice R(int) = 0.180 [ 2794] Vol = 565.5 Cell: 10.382 7.371 7.390 90.22 90.18 90.01 Volume: 565.51 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.196 MONOCLINIC I-lattice R(int) = 0.179 [ 2781] Vol = 565.5 Cell: 7.362 7.345 10.458 90.02 90.19 89.81 Volume: 565.51 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.250 MONOCLINIC C-lattice R(int) = 0.177 [ 2811] Vol = 565.5 Cell: 10.382 10.458 7.345 90.02 134.84 90.12 Volume: 565.51 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) = 0.115 [ 1829] Vol = 282.8 Cell: 7.345 7.360 7.362 119.74 90.19 119.84 Volume: 282.76 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 2026 0 2674 2664 4009 N (int>3sigma) = 0 0 0 0 321 0 614 615 897 Mean intensity = 0.0 0.0 0.0 0.0 0.9 0.0 20.9 20.4 20.2 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.7 4.6 4.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.828 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 25 25 295 776 N I>3s 0 0 0 189 0.0 0.0 -0.0 1.3 0.4 0.4 0.1 2.4 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 0.248 3504 Fd-3m 1 1 227 C N N N N 37 2284 0.248 3568 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.382274 10.457674 10.417134 90.1514 89.8709 90.1203 ZERR 1.00 0.005794 0.000961 0.010478 0.0960 0.0034 0.0051 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 822260- 88718 442 417 48 8.7 328471.15 30.07 0.158 0.173 85996- 2452 519 498 48 10.4 11681.30 4.34 0.315 0.181 2417- 1379 722 716 48 14.9 1916.56 2.05 0.850 0.970 1331- 927 559 555 48 11.6 1068.88 1.34 0.741 0.862 926- 720 431 426 48 8.9 814.92 1.20 0.709 0.714 720- 535 425 419 48 8.7 602.33 0.94 0.686 0.808 526- 419 327 325 48 6.8 455.44 0.82 0.689 0.800 418- 269 227 226 48 4.7 357.35 0.71 0.663 0.802 269- 120 262 261 48 5.4 188.49 0.50 0.852 1.282 113- -337 166 166 54 3.1 24.91 0.12 0.979 3.410 ------------------------------------------------------------------------------------------- 822260- -337 4080 4009 486 8.2 36327.48 4.59 0.177 0.186 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-1.14 986 966 48 20.1 74976.85 8.84 0.189 0.218 0.028 1.14-0.89 709 698 48 14.5 40576.19 4.67 0.175 0.181 0.053 0.89-0.76 594 585 48 12.2 32503.35 3.96 0.153 0.163 0.073 0.76-0.69 510 504 51 9.9 21117.95 3.09 0.156 0.171 0.084 0.69-0.63 401 397 49 8.1 17406.73 2.64 0.199 0.220 0.099 0.63-0.59 306 300 50 6.0 9643.45 1.95 0.226 0.226 0.128 0.58-0.55 225 215 48 4.5 13645.52 2.39 0.093 0.101 0.112 0.55-0.52 146 145 48 3.0 5396.61 1.45 0.110 0.107 0.169 0.52-0.49 125 122 49 2.5 11439.24 2.25 0.075 0.077 0.117 0.49-0.45 78 77 47 1.6 4075.07 1.13 0.453 0.527 0.199 ------------------------------------------------------------------------------------------------------ inf-0.45 4080 4009 486 8.2 36327.48 4.59 0.177 0.186 0.052 inf-0.65 3067 3020 225 13.4 44086.89 5.35 0.179 0.197 0.046 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-1.14 966 48 48 100.0 20.1 74976.85 35.14 0.189 0.008 1.14-0.89 698 48 48 100.0 14.5 40576.19 15.22 0.175 0.019 0.89-0.76 585 48 48 100.0 12.2 32503.35 12.68 0.153 0.030 0.76-0.69 504 51 51 100.0 9.9 21117.95 9.20 0.156 0.033 0.69-0.63 397 51 49 96.1 8.1 17406.73 7.43 0.199 0.045 0.63-0.59 300 56 50 89.3 6.0 9643.45 4.67 0.226 0.057 0.58-0.55 215 55 48 87.3 4.5 13645.52 5.06 0.093 0.056 0.55-0.52 145 65 48 73.8 3.0 5396.61 2.53 0.110 0.090 0.52-0.49 122 81 49 60.5 2.5 11439.24 3.59 0.075 0.076 0.49-0.45 77 146 47 32.2 1.6 4075.07 1.42 0.453 0.902 -------------------------------------------------------------------------------------------- inf-0.45 4009 649 486 74.9 8.2 36327.48 15.71 0.177 0.027 inf-0.65 3020 227 225 99.1 13.4 44086.89 19.19 0.179 0.018 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.066378 0.013057 -0.008885 ( 0.000011 0.000012 0.000012 ) 0.014631 0.065198 -0.013125 ( 0.000010 0.000011 0.000011 ) 0.006100 -0.014608 -0.066261 ( 0.000013 0.000015 0.000014 ) M - matrix: 0.004657 -0.000002 -0.000006 ( 0.000001 0.000001 0.000001 ) -0.000002 0.004635 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000006 -0.000004 0.004642 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.066378 0.013057 -0.008885 ( 0.000011 0.000012 0.000012 ) 0.014631 0.065198 -0.013125 ( 0.000010 0.000011 0.000011 ) 0.006100 -0.014608 -0.066261 ( 0.000013 0.000015 0.000014 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) unit cell: 10.3936(16) 10.419(2) 10.4109(19) 89.953(15) 89.920(14) 89.977(14) V = 1127.4(3) unit cell: 10.4078(5) 10.4078(5) 10.4078(5) 90.0 90.0 90.0 V = 1127.40(9) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.179) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 94.000,100 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-565.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-588.7455 max=1113635.6190 PROFFIT INFO: background sum: min=-50.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=396.0000 max=5594.0000 PROFFIT INFO: num of signal pixels: min=41 max=498 PROFFIT INFO: Inet: min=-941.9929 max=1781817.0000 PROFFIT INFO: sig(Inet): min=57.6010 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.72 max=198.42 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 728 2886 4288 5120 5492 6368 6890 7222 7754 8074 8160 Percent 8.9 35.4 52.5 62.7 67.3 78.0 84.4 88.5 95.0 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4080 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 4080 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1781817- 124037 408 389526.79 75.52 100.00 123971- 3845 408 28760.36 19.34 100.00 3836- 1999 408 2761.97 6.91 97.30 1996- 1165 408 1526.10 3.77 48.77 1164- 792 408 964.42 2.21 12.01 790- 518 408 648.14 1.69 8.33 518- 320 408 413.07 1.17 5.15 320- 144 408 230.59 0.68 0.98 144- 13 408 75.19 0.27 0.00 13- -942 408 -135.79 -0.27 0.00 ------------------------------------------------------------------------------------ 1781817- -942 4080 42477.08 11.13 37.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 408 108608.02 14.98 67.65 1.73- 1.26 408 78380.37 21.03 60.54 1.26- 1.09 408 54917.50 17.74 64.95 1.09- 0.96 408 52084.12 14.62 34.31 0.96- 0.88 408 14741.79 6.60 41.18 0.88- 0.81 408 50424.90 14.25 36.27 0.81- 0.76 408 17935.98 5.65 17.16 0.76- 0.71 408 21037.15 6.92 17.65 0.71- 0.67 408 22898.44 7.68 26.96 0.67- 0.63 408 3742.57 1.85 5.88 ------------------------------------------------------------------------------------ 6.00- 0.63 4080 42477.08 11.13 37.25 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:46:40 2019 Sorting 4080 observations 43 unique observations with > 7.00 F2/sig(F2) 4080 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 99 407 Total number of frames 407 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 4080 observations in 4 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 9 43 Total number of frames 43 967 observations > 7.00 F2/sig(F2) 967 observations in 4 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 9 43 Total number of frames 43 Removing 'redundancy=1' reflections Average redundancy: 18.6 (Out of 967 removed 1 = 966, unique = 52) 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 966 observations in 4 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 9 43 Total number of frames 43 52 unique data precomputed (should be 52) 52 unique data with 966 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 18.6 (Out of 966 removed 0 = 966, unique = 52) 52 unique data precomputed (should be 52) 52 unique data with 966 observations RMS deviation of equivalent data = 0.27838 Rint = 0.19878 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19288, wR= 0.26349 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09430, wR= 0.14766, Acormin=0.577, Acormax=1.371, Acor_av=1.031 F test: Probability=1.000, F= 4.160 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08933, wR= 0.14043, Acormin=0.530, Acormax=1.432, Acor_av=1.002 F test: Probability=0.943, F= 1.111 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08161, wR= 0.13918, Acormin=0.597, Acormax=1.465, Acor_av=1.033 F test: Probability=1.000, F= 1.322 Trying model 4 (ne=4, no=1)... Results: Rint= 0.07895, wR= 0.12882, Acormin=0.539, Acormax=1.560, Acor_av=1.006 F test: Probability=0.826, F= 1.065 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07329, wR= 0.12038, Acormin=0.577, Acormax=1.691, Acor_av=1.014 F test: Probability=0.999, F= 1.226 Final absorption model (ne=4, no=3): Rint= 0.07329, Acormin=0.577, Acormax=1.691, Acor_av=1.014 Combined refinement in use Rint: 0.20096 There are 43 active scales (one needs to be fixed) Refinement control: frame scale #12 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 66 pars with 2211 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.27838 Using Levenberg-Marquardt: 0.00010 New wR= 0.13629 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19878 with corrections 0.09632 Rint for all data: 0.20096 with corrections 0.09900 3 observations identified as outliers and rejected Cycle 2 wR= 0.11960 Using Levenberg-Marquardt: 0.00001 New wR= 0.11075 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19534 with corrections 0.07077 Rint for all data: 0.20096 with corrections 0.08013 2 observations identified as outliers and rejected Cycle 3 wR= 0.08748 Using Levenberg-Marquardt: 0.00000 New wR= 0.07759 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19348 with corrections 0.05635 Rint for all data: 0.20096 with corrections 0.06749 0 observations identified as outliers and rejected Cycle 4 wR= 0.07759 Using Levenberg-Marquardt: 0.00000 New wR= 0.07746 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19348 with corrections 0.05581 Rint for all data: 0.20096 with corrections 0.06706 0 observations identified as outliers and rejected Cycle 5 wR= 0.07746 Using Levenberg-Marquardt: 0.00000 New wR= 0.07755 Using Levenberg-Marquardt: 0.00000 New wR= 0.07755 Using Levenberg-Marquardt: 0.00000 New wR= 0.07755 Using Levenberg-Marquardt: 0.00001 New wR= 0.07755 Using Levenberg-Marquardt: 0.00010 New wR= 0.07755 Using Levenberg-Marquardt: 0.00100 New wR= 0.07755 Using Levenberg-Marquardt: 0.01000 New wR= 0.07755 Using Levenberg-Marquardt: 0.10000 New wR= 0.07754 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19348 with corrections 0.05603 Rint for all data: 0.20096 with corrections 0.06731 Final wR= 0.07754 Final frame scales: Min= 0.8263 Max= 1.1876 Final absorption correction factors: Amin= 0.5173 Amax= 1.5668 PROFFIT INFO: Inet (after scale3 abspack): min=-870.3287 max=1266539.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=48.1361 max=23636.1699 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/103 4080 reflections read from tmp file 180 reflections are rejected (178 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 4 5 5 5 3 5 2 131 Initial Chi^2= 0.53584 Cycle 1, Chi^2= 1.05108 Current error model SIG(F2)^2 = 73.10*I_RAW + 8.08*I_BACK+(0.03550*)^2 Cycle 2, Chi^2= 1.02869 Current error model SIG(F2)^2 = 90.67*I_RAW + 5.12*I_BACK+(0.03023*)^2 Cycle 3, Chi^2= 1.01086 Current error model SIG(F2)^2 = 97.62*I_RAW + 4.31*I_BACK+(0.02874*)^2 Cycle 4, Chi^2= 1.00316 Current error model SIG(F2)^2 = 99.83*I_RAW + 4.10*I_BACK+(0.02842*)^2 Cycle 5, Chi^2= 1.00081 Current error model SIG(F2)^2 = 100.43*I_RAW + 4.05*I_BACK+(0.02836*)^2 Cycle 6, Chi^2= 1.00020 Current error model SIG(F2)^2 = 100.58*I_RAW + 4.04*I_BACK+(0.02834*)^2 Final Chi^2= 1.00020 Final error model SIG(F2)^2 = 100.58*I_RAW + 4.04*I_BACK+(0.02834*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1266539- 115154 408 376479.97 28.60 100.00 114804- 3461 408 28880.86 11.94 100.00 3452- 1972 408 2645.74 5.56 97.79 1967- 1130 408 1484.62 3.62 54.41 1129- 758 408 917.75 2.50 13.97 758- 503 408 625.45 2.17 9.56 502- 311 408 405.06 1.85 8.33 310- 141 408 225.48 1.36 1.96 141- 13 408 75.41 0.69 0.00 13- -870 408 -132.79 -0.58 0.00 ------------------------------------------------------------------------------------ 1266539- -870 4080 41160.75 5.77 38.60 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 408 107283.25 9.40 70.10 1.73- 1.26 408 76988.14 8.65 61.27 1.26- 1.09 408 54825.40 7.45 67.16 1.09- 0.96 408 48945.95 6.24 35.54 0.96- 0.88 408 15638.46 4.35 44.12 0.88- 0.81 408 46712.72 7.07 37.99 0.81- 0.76 408 16774.14 3.50 17.16 0.76- 0.71 408 19236.42 4.52 18.38 0.71- 0.67 408 21616.81 4.90 28.19 0.67- 0.63 408 3586.26 1.65 6.13 ------------------------------------------------------------------------------------ 6.00- 0.63 4080 41160.75 5.77 38.60 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 408 107283.25 9.40 70.10 6.00- 1.26 816 92135.70 9.02 65.69 6.00- 1.09 1224 79698.93 8.50 66.18 6.00- 0.96 1632 72010.69 7.93 58.52 6.00- 0.88 2040 60736.24 7.22 55.64 6.00- 0.81 2448 58398.99 7.19 52.70 6.00- 0.76 2856 52452.58 6.66 47.62 6.00- 0.71 3264 48300.56 6.40 43.96 6.00- 0.67 3672 45335.70 6.23 42.21 6.00- 0.63 4080 41160.75 5.77 38.60 ------------------------------------------------------------------------------------ 6.00- 0.63 4080 41160.75 5.77 38.60 Scale applied to data: s=0.789552 (maximum obs:1266539.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.067; Rsigma 0.040: data 4080 -> merged 162 With outlier rejection... Rint 0.055; Rsigma 0.040: data 4059 -> merged 162 Rejected total: 21, method kkm 14, method Blessing 7 Completeness direct cell (a, b, c) = (10.408, 10.408, 10.408), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626476, 6.008947 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.76 14 14 26.57 100.00 372 1.73 - 1.27 14 14 29.36 100.00 411 1.26 - 1.06 14 14 33.00 100.00 462 1.05 - 0.97 14 14 28.64 100.00 401 0.95 - 0.88 14 14 29.93 100.00 419 0.87 - 0.81 14 14 26.64 100.00 373 0.80 - 0.76 14 14 28.21 100.00 395 0.76 - 0.72 14 14 23.50 100.00 329 0.72 - 0.69 14 14 25.43 100.00 356 0.69 - 0.65 19 19 21.58 100.00 410 --------------------------------------------------------------- 7.36 - 0.65 145 145 27.09 100.00 3928 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:46:39 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.375815 7.360342 7.370613 120.1801 120.1007 89.5854 4009 Reflections read from file xs2212a.hkl 4009 Reflections used for space-group determination (up to diffraction limit of 0.46A); mean (I/sigma) = 4.59 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2007 2009 2026 2011 3021 2663 2674 4009 N (int>3sigma) = 0 218 237 321 219 388 606 614 897 Mean intensity = 0.0 0.6 0.7 0.9 0.6 0.7 19.8 20.9 20.2 Mean int/sigma = 0.0 1.4 1.4 1.9 1.4 1.6 4.5 4.7 4.6 Lattice type: P chosen Volume: 282.76 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.360 7.362 119.74 90.19 119.84 Niggli form: a.a = 53.955 b.b = 54.175 c.c = 54.199 b.c = -26.880 a.c = -0.181 a.b = -26.902 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.319 CUBIC F-lattice R(int) = 0.249 [ 3771] Vol = 1131.0 Cell: 10.382 10.458 10.417 90.15 89.87 90.12 Volume: 1131.03 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.318 RHOMBOHEDRAL R-lattice R(int) = 0.225 [ 3337] Vol = 848.3 Cell: 7.360 7.345 18.088 89.83 90.35 119.84 Volume: 848.27 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.318 RHOMBOHEDRAL R-lattice R(int) = 0.226 [ 1078] Vol = 848.3 Trigonal Cell: 7.360 7.345 18.088 89.83 90.35 119.84 Volume: 848.27 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.529 TETRAGONAL I-lattice R(int) = 0.227 [ 3383] Vol = 565.5 Cell: 7.371 7.390 10.382 89.82 89.99 90.22 Volume: 565.51 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.520 TETRAGONAL I-lattice R(int) = 0.227 [ 3383] Vol = 565.5 Cell: 7.371 7.390 10.382 89.82 89.99 90.22 Volume: 565.51 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.364 ORTHORHOMBIC I-lattice R(int) = 0.186 [ 3312] Vol = 565.5 Cell: 7.371 10.382 7.390 89.82 89.78 90.01 Volume: 565.51 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.231 MONOCLINIC I-lattice R(int) = 0.180 [ 2794] Vol = 565.5 Cell: 10.382 7.371 7.390 90.22 90.18 90.01 Volume: 565.51 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.196 MONOCLINIC I-lattice R(int) = 0.179 [ 2781] Vol = 565.5 Cell: 7.362 7.345 10.458 90.02 90.19 89.81 Volume: 565.51 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.250 MONOCLINIC C-lattice R(int) = 0.177 [ 2811] Vol = 565.5 Cell: 10.382 10.458 7.345 90.02 134.84 90.12 Volume: 565.51 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) = 0.115 [ 1829] Vol = 282.8 Cell: 7.345 7.360 7.362 119.74 90.19 119.84 Volume: 282.76 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 2026 0 2674 2664 4009 N (int>3sigma) = 0 0 0 0 321 0 614 615 897 Mean intensity = 0.0 0.0 0.0 0.0 0.9 0.0 20.9 20.4 20.2 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.7 4.6 4.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.828 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 25 25 295 776 N I>3s 0 0 0 189 0.0 0.0 -0.0 1.3 0.4 0.4 0.1 2.4 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 0.248 3504 Fd-3m 1 1 227 C N N N N 37 2284 0.248 3568 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.382274 10.457674 10.417134 90.1514 89.8709 90.1203 ZERR 1.00 0.005794 0.000961 0.010478 0.0960 0.0034 0.0051 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1147398- 89318 498 486 27 18.0 326330.33 26.83 0.051 0.060 74716- 1690 770 764 27 28.3 5165.19 7.54 0.097 0.118 1656- 757 801 799 27 29.6 1107.00 2.74 0.230 0.301 680- 324 809 809 27 30.0 487.59 1.84 0.382 0.541 312- 64 577 576 27 21.3 217.63 1.14 0.602 0.971 63- -236 625 625 27 23.1 8.14 0.18 0.954 3.341 ------------------------------------------------------------------------------------------- 1147398- -236 4080 4059 162 25.1 40392.25 5.73 0.055 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-1.27 788 782 27 29.0 92327.73 9.17 0.046 0.050 0.032 1.26-0.97 822 819 27 30.3 51272.69 6.76 0.052 0.068 0.036 0.97-0.81 840 836 29 28.8 29955.04 5.56 0.055 0.066 0.047 0.80-0.73 706 705 27 26.1 17099.52 3.85 0.081 0.096 0.060 0.72-0.67 618 617 27 22.9 18442.68 4.27 0.091 0.115 0.067 0.66-0.63 306 300 25 12.0 4276.07 1.76 0.127 0.100 0.124 ------------------------------------------------------------------------------------------------------ inf-0.63 4080 4059 162 25.1 40392.25 5.73 0.055 0.064 0.040 inf-0.65 3943 3927 144 27.3 41517.21 5.85 0.055 0.063 0.040 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-1.27 782 27 27 100.0 29.0 92327.73 47.72 0.046 0.009 1.26-0.97 819 27 27 100.0 30.3 51272.69 35.49 0.052 0.008 0.97-0.81 836 29 29 100.0 28.8 29955.04 30.19 0.055 0.011 0.80-0.73 705 27 27 100.0 26.1 17099.52 17.97 0.081 0.014 0.72-0.67 617 27 27 100.0 22.9 18442.68 22.20 0.091 0.015 0.66-0.63 300 25 25 100.0 12.0 4276.07 6.41 0.127 0.040 -------------------------------------------------------------------------------------------- inf-0.63 4059 162 162 100.0 25.1 40392.25 29.54 0.055 0.011 inf-0.65 3927 144 144 100.0 27.3 41517.21 30.36 0.055 0.010 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:48:03 2019) ID: 3668; threads 39; handles 811; mem 515784.00 (1197524.00)kB; time: 1w 4d 23h 58m 51s MEMORY INFO: Memory PF:280.0, Ph:622.0, V:1168.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:503.7,peak PF: 700.2, WS: 471.5, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:282.0, Ph:624.0, V:1170.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:505.5,peak PF: 700.2, WS: 473.3, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:48:03 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000086 0.000065 0.000087 ) 0.064809 0.092374 0.027273 ( 0.000103 0.000078 0.000104 ) 0.045523 0.057900 0.132205 ( 0.000122 0.000094 0.000124 ) 7.38096 ( 0.00671 ) 7.36649 ( 0.00728 ) 7.42630 ( 0.00831 ) 120.52449 ( 0.11226 ) 120.40327 ( 0.10774 ) 89.27095 ( 0.07682 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:48:03 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000086 0.000065 0.000087 ) 0.064809 0.092374 0.027273 ( 0.000103 0.000078 0.000104 ) 0.045523 0.057900 0.132205 ( 0.000122 0.000094 0.000124 ) M - matrix: 0.013763 0.004504 0.009152 ( 0.000023 0.000015 0.000020 ) 0.004504 0.013962 0.009328 ( 0.000015 0.000019 0.000018 ) 0.009152 0.009328 0.018530 ( 0.000020 0.000018 0.000033 ) unit cell: 7.381(7) 7.366(7) 7.426(8) 120.52(11) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 238 peaks identified as outliers and rejected 238 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 238 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 238 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.79 | 24 | 1.006 ( 0.048) | 1.013 ( 0.135) | 0.894 ( 0.352) | 0.79- 0.69 | 24 | 0.997 ( 0.042) | 1.000 ( 0.131) | 1.289 ( 0.496) | 0.69- 0.63 | 22 | 0.976 ( 0.051) | 0.906 ( 0.101) | 1.172 ( 0.435) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 238 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb PROFFITPEAK info: 421 peaks in the peak location table UB fit with 46 obs out of 238 (total:238,skipped:0) (19.33%) UB - matrix: 0.086322 -0.045974 0.017116 ( 0.000473 0.000165 0.000229 ) 0.064318 0.092941 0.027760 ( 0.000633 0.000220 0.000306 ) 0.045617 0.058321 0.132889 ( 0.000830 0.000289 0.000401 ) M - matrix: 0.013669 0.004670 0.009325 ( 0.000138 0.000083 0.000117 ) 0.004670 0.014153 0.009543 ( 0.000083 0.000055 0.000055 ) 0.009325 0.009543 0.018723 ( 0.000117 0.000055 0.000108 ) unit cell: 7.47(3) 7.36(3) 7.42(3) 120.7(5) 120.4(5) 89.5(4) V = 285(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 4, #refl in peak table: 238 #indexed refl 216, indexation with best UB: 90.7563% Lattice: 7.4072 7.3556 7.3610 120.005 120.354 89.764 282.632 Rotation: -22.660 24.759 -35.022 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 227 obs out of 238 (total:238,skipped:0) (95.38%) UB - matrix: 0.087760 -0.044390 0.012681 ( 0.000052 0.000055 0.000059 ) 0.061495 0.094382 0.026268 ( 0.000060 0.000065 0.000069 ) 0.049386 0.055440 0.133261 ( 0.000059 0.000063 0.000067 ) M - matrix: 0.013922 0.004646 0.009310 ( 0.000013 0.000010 0.000011 ) 0.004646 0.013952 0.009304 ( 0.000010 0.000015 0.000012 ) 0.009310 0.009304 0.018609 ( 0.000011 0.000012 0.000018 ) unit cell: 7.369(4) 7.355(5) 7.360(5) 120.01(7) 120.09(6) 89.95(5) V = 281.8(3) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) 238 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1316 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 223 peaks identified as outliers and rejected 223 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 223 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 223 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 2.38 | 22 | 0.899 ( 0.094) | 0.905 ( 0.131) | 0.958 ( 0.493) | 2.38- 1.83 | 22 | 0.900 ( 0.110) | 0.921 ( 0.154) | 0.939 ( 0.269) | 1.76- 1.58 | 22 | 0.887 ( 0.115) | 0.904 ( 0.161) | 0.806 ( 0.264) | 1.58- 1.35 | 22 | 0.954 ( 0.082) | 0.983 ( 0.130) | 0.791 ( 0.395) | 1.35- 1.19 | 22 | 0.935 ( 0.082) | 0.954 ( 0.100) | 0.903 ( 0.428) | 1.19- 1.00 | 22 | 0.962 ( 0.087) | 0.981 ( 0.123) | 0.884 ( 0.304) | 1.00- 0.88 | 22 | 0.988 ( 0.064) | 0.995 ( 0.081) | 1.052 ( 0.398) | 0.88- 0.79 | 22 | 0.993 ( 0.048) | 0.994 ( 0.129) | 0.938 ( 0.310) | 0.79- 0.69 | 22 | 0.975 ( 0.044) | 0.932 ( 0.088) | 1.196 ( 0.465) | 0.69- 0.63 | 25 | 0.933 ( 0.047) | 0.852 ( 0.068) | 1.275 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 0.63 | 223 | 0.942 ( 0.089) | 0.941 ( 0.128) | 0.978 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) UB - matrix: 0.088106 -0.044293 0.012828 ( 0.000028 0.000032 0.000033 ) 0.061394 0.094519 0.026063 ( 0.000022 0.000026 0.000027 ) 0.049283 0.055378 0.133130 ( 0.000021 0.000024 0.000025 ) M - matrix: 0.013961 0.004630 0.009291 ( 0.000006 0.000004 0.000005 ) 0.004630 0.013962 0.009268 ( 0.000004 0.000006 0.000005 ) 0.009291 0.009268 0.018567 ( 0.000005 0.000005 0.000007 ) unit cell: 7.351(2) 7.341(2) 7.3536(18) 119.91(3) 120.04(3) 89.95(2) V = 280.88(13) OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 UB - matrix: 0.087896 -0.044356 0.012683 ( 0.000021 0.000024 0.000025 ) 0.061495 0.094417 0.026185 ( 0.000020 0.000022 0.000024 ) 0.049387 0.055447 0.133218 ( 0.000019 0.000022 0.000023 ) M - matrix: 0.013946 0.004646 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013956 0.009296 ( 0.000004 0.000005 0.000004 ) 0.009304 0.009296 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3589(17) 7.3517(18) 7.3584(16) 119.99(2) 120.05(2) 89.96(2) V = 281.42(11) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087896 -0.044356 0.012683 ( 0.000021 0.000024 0.000025 ) 0.061495 0.094417 0.026185 ( 0.000020 0.000022 0.000024 ) 0.049387 0.055447 0.133218 ( 0.000019 0.000022 0.000023 ) M - matrix: 0.013946 0.004646 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013956 0.009296 ( 0.000004 0.000005 0.000004 ) 0.009304 0.009296 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3589(17) 7.3517(18) 7.3584(16) 119.99(2) 120.05(2) 89.96(2) V = 281.42(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) 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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 223 peaks identified as outliers and rejected 223 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 223 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 223 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 22 | 0.868 ( 0.103) | 0.880 ( 0.128) | 0.911 ( 0.399) | 2.38- 1.83 | 22 | 0.907 ( 0.104) | 0.924 ( 0.157) | 0.918 ( 0.259) | 1.76- 1.59 | 22 | 0.880 ( 0.117) | 0.891 ( 0.164) | 0.729 ( 0.225) | 1.58- 1.45 | 22 | 0.947 ( 0.083) | 0.969 ( 0.129) | 0.883 ( 0.461) | 1.45- 1.19 | 22 | 0.926 ( 0.075) | 0.944 ( 0.084) | 0.839 ( 0.422) | 1.19- 1.06 | 22 | 0.980 ( 0.083) | 1.000 ( 0.124) | 0.894 ( 0.363) | 1.01- 0.88 | 22 | 0.983 ( 0.064) | 1.014 ( 0.078) | 1.039 ( 0.371) | 0.88- 0.79 | 22 | 0.991 ( 0.048) | 0.987 ( 0.128) | 0.966 ( 0.330) | 0.79- 0.69 | 22 | 0.976 ( 0.044) | 0.935 ( 0.090) | 1.283 ( 0.490) | 0.69- 0.63 | 25 | 0.933 ( 0.048) | 0.854 ( 0.073) | 1.273 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 223 | 0.939 ( 0.090) | 0.939 ( 0.130) | 0.977 ( 0.421) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 93 | 0.982 ( 0.036) | 1.029 ( 0.069) | 1.114 ( 0.489) | 10.3-14.9 | 93 | 0.983 ( 0.044) | 1.039 ( 0.069) | 1.172 ( 0.538) | 14.9-19.0 | 93 | 0.992 ( 0.219) | 1.019 ( 0.097) | 1.201 ( 1.134) | 19.0-23.6 | 93 | 0.959 ( 0.057) | 1.002 ( 0.081) | 0.932 ( 0.420) | 23.6-27.4 | 93 | 0.959 ( 0.063) | 0.992 ( 0.094) | 0.942 ( 0.422) | 27.5-32.6 | 93 | 0.946 ( 0.084) | 0.959 ( 0.113) | 0.929 ( 0.443) | 32.6-36.4 | 93 | 0.917 ( 0.163) | 0.900 ( 0.132) | 1.078 ( 0.653) | 36.4-39.0 | 93 | 0.876 ( 0.091) | 0.843 ( 0.122) | 1.010 ( 0.501) | 39.0-42.0 | 93 | 0.895 ( 0.092) | 0.838 ( 0.119) | 1.053 ( 0.482) | 42.0-50.1 | 90 | 0.872 ( 0.119) | 0.794 ( 0.137) | 0.957 ( 0.459) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 927 | 0.938 ( 0.119) | 0.942 ( 0.136) | 1.039 ( 0.599) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.14 e2 dimension: a=-0.0072 b=1.25 e3 dimension: a=0.0011 b=1.07 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3814 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:48:18 2019 PROFFITMAIN - Started at Wed Aug 21 13:48:18 2019 OTKP changes: 349 2 3 4 OTKP changes: 349 2 3 4 OTKP changes: 349 2 3 4 UB - matrix: 0.087741 -0.045993 0.016766 ( 0.000081 0.000064 0.000083 ) 0.063149 0.092370 0.026722 ( 0.000091 0.000073 0.000093 ) 0.045310 0.057607 0.131908 ( 0.000095 0.000076 0.000097 ) M - matrix: 0.013739 0.004408 0.009135 ( 0.000020 0.000013 0.000016 ) 0.004408 0.013966 0.009296 ( 0.000013 0.000017 0.000015 ) 0.009135 0.009296 0.018395 ( 0.000016 0.000015 0.000026 ) UB fit with 407 obs out of 927 (total:927,skipped:0) (43.91%) unit cell: 7.396(6) 7.370(7) 7.438(7) 120.79(10) 120.34(9) 88.70(7) V = 285.0(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 201 obs out of 212 (total:212,skipped:0) (94.81%) UB - matrix: 0.087628 -0.046170 0.017193 ( 0.000107 0.000067 0.000101 ) 0.064541 0.092382 0.027068 ( 0.000089 0.000055 0.000084 ) 0.045783 0.057755 0.132018 ( 0.000107 0.000066 0.000100 ) M - matrix: 0.013940 0.004561 0.009298 ( 0.000024 0.000014 0.000018 ) 0.004561 0.014002 0.009332 ( 0.000014 0.000014 0.000014 ) 0.009298 0.009332 0.018457 ( 0.000018 0.000014 0.000027 ) unit cell: 7.373(7) 7.362(7) 7.438(7) 120.53(9) 120.46(10) 89.14(7) V = 283.4(4) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.165) HKL list info: 1285 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087480 -0.046172 0.017356 ( 0.000100 0.000062 0.000093 ) 0.064777 0.092360 0.027257 ( 0.000086 0.000053 0.000080 ) 0.045691 0.057812 0.132116 ( 0.000104 0.000064 0.000096 ) M - matrix: 0.013937 0.004585 0.009320 ( 0.000023 0.000013 0.000018 ) 0.004585 0.014004 0.009354 ( 0.000013 0.000014 0.000013 ) 0.009320 0.009354 0.018499 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.379(6) 7.366(6) 7.435(6) 120.52(9) 120.46(9) 89.21(7) V = 283.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 204 obs out of 212 (total:212,skipped:0) (96.23%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.117994 0.039001 0.078634 ( 0.000076 0.000047 0.000070 ) 0.000082 0.111544 0.056279 ( 0.000080 0.000050 0.000074 ) -0.000026 -0.000075 0.095377 ( 0.000090 0.000056 0.000083 ) M - matrix: 0.013923 0.004611 0.009280 ( 0.000018 0.000011 0.000014 ) 0.004611 0.013963 0.009337 ( 0.000011 0.000012 0.000011 ) 0.009280 0.009337 0.018447 ( 0.000014 0.000011 0.000021 ) UB fit with 207 obs out of 212 (total:212,skipped:0) (97.64%) unit cell: 7.374(5) 7.380(5) 7.433(8) 120.48(9) 120.25(9) 89.46(6) V = 284.2(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) UB - matrix: 0.087805 -0.044307 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094150 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055800 0.133162 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004659 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004659 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009313 0.018586 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3552(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 238 1 1 1 OTKP changes: 238 1 1 1 OTKP changes: 238 1 1 1 UB - matrix: 0.087792 -0.044305 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094149 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055807 0.133151 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009314 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009314 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087792 -0.044305 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094149 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055807 0.133151 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009314 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009314 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 238 obs out of 238 (total:238,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: 0.087792 -0.044305 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094149 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055807 0.133151 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009314 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009314 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) UB - matrix: 0.087903 -0.044369 0.012678 ( 0.000021 0.000024 0.000026 ) 0.061483 0.094414 0.026172 ( 0.000019 0.000022 0.000023 ) 0.049390 0.055433 0.133214 ( 0.000017 0.000020 0.000021 ) M - matrix: 0.013947 0.004643 0.009303 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013955 0.009293 ( 0.000004 0.000005 0.000004 ) 0.009303 0.009293 0.018592 ( 0.000004 0.000004 0.000006 ) unit cell: 7.3585(17) 7.3510(18) 7.3581(15) 119.98(2) 120.05(2) 89.95(2) V = 281.39(11) OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1296 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087903 -0.044369 0.012678 ( 0.000021 0.000024 0.000026 ) 0.061483 0.094414 0.026172 ( 0.000019 0.000022 0.000023 ) 0.049390 0.055433 0.133214 ( 0.000017 0.000020 0.000021 ) M - matrix: 0.013947 0.004643 0.009303 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013955 0.009293 ( 0.000004 0.000005 0.000004 ) 0.009303 0.009293 0.018592 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3585(17) 7.3510(18) 7.3581(15) 119.98(2) 120.05(2) 89.95(2) V = 281.39(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* UB - matrix: 0.118100 0.039327 0.078777 ( 0.000021 0.000024 0.000026 ) 0.000003 0.111393 0.055619 ( 0.000011 0.000012 0.000013 ) -0.000002 0.000003 0.096401 ( 0.000023 0.000027 0.000029 ) M - matrix: 0.013948 0.004645 0.009304 ( 0.000005 0.000003 0.000004 ) 0.004645 0.013955 0.009294 ( 0.000003 0.000003 0.000004 ) 0.009304 0.009294 0.018592 ( 0.000004 0.000004 0.000007 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3582(16) 7.3514(13) 7.358(3) 119.98(3) 120.05(3) 89.965(17) V = 281.39(12) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117649 0.038634 0.078493 ( 0.000040 0.000039 0.000044 ) -0.000001 0.111483 0.056071 ( 0.000026 0.000025 0.000028 ) -0.000050 -0.000126 0.096155 ( 0.000028 0.000027 0.000030 ) M - matrix: 0.013841 0.004545 0.009230 ( 0.000009 0.000006 0.000007 ) 0.004545 0.013921 0.009271 ( 0.000006 0.000006 0.000006 ) 0.009230 0.009271 0.018551 ( 0.000007 0.000006 0.000010 ) UB fit with 920 obs out of 927 (total:927,skipped:0) (99.24%) unit cell: 7.375(3) 7.360(2) 7.370(3) 120.18(3) 120.10(4) 89.58(3) V = 282.69(16) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 89 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof 4125 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:48:25 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.165) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-565.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-588.7526 max=1114639.8689 PROFFIT INFO: background sum: min=-77.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=394.0000 max=5571.0000 PROFFIT INFO: num of signal pixels: min=41 max=497 PROFFIT INFO: Inet: min=-942.0042 max=1783423.8750 PROFFIT INFO: sig(Inet): min=57.4333 max=24370.4648 PROFFIT INFO: Inet/sig(Inet): min=-1.72 max=198.43 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 365 1458 2167 2589 2772 3217 3482 3649 3916 4080 4125 Percent 8.8 35.3 52.5 62.8 67.2 78.0 84.4 88.5 94.9 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4125 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 4125 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1783424- 126052 412 393286.36 75.92 100.00 124374- 3848 412 29383.98 19.46 100.00 3846- 2012 412 2777.53 6.97 97.33 2012- 1173 412 1535.60 3.79 49.03 1172- 791 412 969.71 2.25 12.62 790- 519 412 651.09 1.68 7.77 519- 319 412 413.93 1.18 4.85 319- 149 412 232.26 0.69 1.21 148- 16 412 78.36 0.29 0.00 15- -942 417 -130.91 -0.26 0.00 ------------------------------------------------------------------------------------ 1783424- -942 4125 42867.61 11.18 37.24 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 412 96605.84 15.96 69.66 1.75- 1.26 412 93974.38 21.91 59.22 1.26- 1.04 412 55205.15 16.23 50.97 1.04- 0.90 412 36886.83 11.04 38.59 0.90- 0.81 412 26319.28 8.67 31.80 0.81- 0.74 412 37388.99 11.25 37.62 0.74- 0.68 412 26008.68 8.27 25.97 0.68- 0.62 412 23093.27 7.28 23.54 0.62- 0.56 412 19514.14 6.46 20.15 0.56- 0.44 417 14029.49 4.85 15.11 ------------------------------------------------------------------------------------ 6.55- 0.44 4125 42867.61 11.18 37.24 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:48:25 2019 Sorting 4125 observations 90 unique observations with > 7.00 F2/sig(F2) 4125 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 103 411 Total number of frames 411 Maximum number of 90 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 4125 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 20 84 Total number of frames 84 983 observations > 7.00 F2/sig(F2) 983 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 20 84 Total number of frames 84 Removing 'redundancy=1' reflections Average redundancy: 7.5 (Out of 983 removed 30 = 953, 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 953 observations in 4 runs Run # start # end # total # 1 0 20 21 2 0 20 42 3 0 20 63 4 0 20 84 Total number of frames 84 127 unique data precomputed (should be 127) 127 unique data with 953 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.5 (Out of 953 removed 0 = 953, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 953 observations RMS deviation of equivalent data = 0.39164 Rint = 0.35032 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.34962, wR= 0.47793 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26035, wR= 0.35615, Acormin=0.510, Acormax=1.471, Acor_av=1.023 F test: Probability=1.000, F= 1.792 Trying model 2 (ne=2, no=1)... Results: Rint= 0.25053, wR= 0.35118, Acormin=0.529, Acormax=1.487, Acor_av=0.987 F test: Probability=0.853, F= 1.076 Trying model 3 (ne=4, no=0)... Results: Rint= 0.25416, wR= 0.34678, Acormin=0.490, Acormax=1.628, Acor_av=0.973 F test: Probability=0.702, F= 1.038 Trying model 4 (ne=4, no=1)... Results: Rint= 0.23873, wR= 0.33743, Acormin=0.383, Acormax=1.671, Acor_av=0.953 F test: Probability=0.988, F= 1.172 Trying model 5 (ne=4, no=3)... Results: Rint= 0.23637, wR= 0.32472, Acormin=0.272, Acormax=1.768, Acor_av=0.868 F test: Probability=0.563, F= 1.011 Trying model 6 (ne=6, no=0)... Results: Rint= 0.25434, wR= 0.33070, Acormin=0.245, Acormax=1.627, Acor_av=0.926 F test: Probability=0.000, F= 0.870 Trying model 7 (ne=6, no=1)... Results: Rint= 0.23880, wR= 0.31735, Acormin=0.206, Acormax=1.679, Acor_av=0.931 F test: Probability=0.000, F= 0.983 Trying model 8 (ne=6, no=3)... Results: Rint= 0.24312, wR= 0.31339, Acormin=0.157, Acormax=1.808, Acor_av=0.822 F test: Probability=0.000, F= 0.940 Trying model 9 (ne=6, no=5)... Results: Rint= 0.25020, wR= 0.32363, Acormin=0.181, Acormax=2.013, Acor_av=0.749 F test: Probability=0.000, F= 0.875 Trying model 10 (ne=8, no=0)... Results: Rint= 0.26805, wR= 0.32376, Acormin=-0.022, Acormax=1.634, Acor_av=0.830 F test: Probability=0.000, F= 0.767 Trying model 11 (ne=8, no=1)... Results: Rint= 0.31703, wR= 0.36405, Acormin=-0.006, Acormax=1.318, Acor_av=0.613 F test: Probability=0.000, F= 0.546 Trying model 12 (ne=8, no=3)... Results: Rint= 0.32179, wR= 0.37271, Acormin=-0.004, Acormax=0.106, Acor_av=0.040 F test: Probability=0.000, F= 0.525 Trying model 13 (ne=8, no=5)... Results: Rint= 0.29511, wR= 0.34793, Acormin=-0.002, Acormax=0.112, Acor_av=0.042 F test: Probability=0.000, F= 0.616 Trying model 14 (ne=8, no=7)... Results: Rint= 0.23608, wR= 0.30217, Acormin=-0.006, Acormax=0.157, Acor_av=0.044 F test: Probability=0.000, F= 0.943 Final absorption model (ne=4, no=1): Rint= 0.23873, Acormin=0.383, Acormax=1.671, Acor_av=0.953 Combined refinement in use Rint: 0.36441 There are 84 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 1 (17 parameters) Refinement control: 100 pars with 5050 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.39164 Using Levenberg-Marquardt: 0.00010 New wR= 0.22575 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35032 with corrections 0.19603 Rint for all data: 0.36441 with corrections 0.21176 0 observations identified as outliers and rejected Cycle 2 wR= 0.22575 Using Levenberg-Marquardt: 0.00001 New wR= 0.21687 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35032 with corrections 0.18656 Rint for all data: 0.36441 with corrections 0.20236 0 observations identified as outliers and rejected Cycle 3 wR= 0.21687 Using Levenberg-Marquardt: 0.00000 New wR= 0.21490 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35032 with corrections 0.18451 Rint for all data: 0.36441 with corrections 0.20033 0 observations identified as outliers and rejected Cycle 4 wR= 0.21490 Using Levenberg-Marquardt: 0.00000 New wR= 0.21521 Using Levenberg-Marquardt: 0.00000 New wR= 0.21521 Using Levenberg-Marquardt: 0.00001 New wR= 0.21520 Using Levenberg-Marquardt: 0.00010 New wR= 0.21519 Using Levenberg-Marquardt: 0.00100 New wR= 0.21509 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.35032 with corrections 0.18480 Rint for all data: 0.36441 with corrections 0.20062 Final wR= 0.21509 Final frame scales: Min= 0.8504 Max= 3.8131 Final absorption correction factors: Amin= 0.3560 Amax= 1.7241 PROFFIT INFO: Inet (after scale3 abspack): min=-1657.9749 max=1613371.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=43.5449 max=34843.8477 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/104 4125 reflections read from tmp file 1029 reflections are rejected (974 as outliers, 55 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 75 52 32 32 40 25 23 24 122 Initial Chi^2= 2.23273 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.85481 Current error model SIG(F2)^2 = 474.90*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 405.95*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 405.95*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1613371- 110648 412 352404.15 32.06 100.00 110336- 3730 412 25843.20 6.87 82.28 3676- 1863 412 2490.54 2.65 29.61 1859- 1126 412 1462.89 1.98 16.50 1122- 715 412 894.07 1.36 1.21 715- 470 412 583.30 1.12 0.24 470- 282 412 368.78 1.04 0.97 281- 136 412 208.91 0.83 0.24 136- 13 412 71.01 0.49 0.24 13- -1658 417 -153.65 -0.33 0.00 ------------------------------------------------------------------------------------ 1613371- -1658 4125 38370.57 4.80 23.10 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 412 89509.48 10.95 53.64 1.75- 1.26 412 88924.85 9.37 40.29 1.26- 1.04 412 50854.40 6.22 32.77 1.04- 0.90 412 34727.13 4.03 17.23 0.90- 0.81 412 22896.64 3.25 13.59 0.81- 0.74 412 33507.08 4.04 19.90 0.74- 0.68 412 21675.48 3.05 14.08 0.68- 0.62 412 18183.62 2.74 13.83 0.62- 0.56 412 14484.91 2.45 14.81 0.56- 0.44 417 9294.93 1.92 11.03 ------------------------------------------------------------------------------------ 6.55- 0.44 4125 38370.57 4.80 23.10 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 412 89509.48 10.95 53.64 6.55- 1.26 824 89217.17 10.16 46.97 6.55- 1.04 1236 76429.58 8.85 42.23 6.55- 0.90 1648 66003.97 7.64 35.98 6.55- 0.81 2060 57382.50 6.76 31.50 6.55- 0.74 2472 53403.27 6.31 29.57 6.55- 0.68 2884 48870.72 5.85 27.36 6.55- 0.62 3296 45034.84 5.46 25.67 6.55- 0.56 3708 41640.40 5.12 24.46 6.55- 0.44 4125 38370.57 4.80 23.10 ------------------------------------------------------------------------------------ 6.55- 0.44 4125 38370.57 4.80 23.10 Scale applied to data: s=0.619820 (maximum obs:1613371.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.201; Rsigma 0.050: data 4125 -> merged 487 With outlier rejection... Rint 0.190; Rsigma 0.050: data 4058 -> merged 487 Rejected total: 67, method kkm 46, method Blessing 21 Completeness direct cell (a, b, c) = (6.563, 6.563, 6.563), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445529, 6.563052 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.59 22 22 21.68 100.00 477 1.55 - 1.22 22 22 19.27 100.00 424 1.20 - 1.02 22 22 17.00 100.00 374 1.02 - 0.92 22 22 13.91 100.00 306 0.92 - 0.84 22 22 14.23 100.00 313 0.84 - 0.79 22 22 11.50 100.00 253 0.79 - 0.75 22 22 11.73 100.00 258 0.75 - 0.71 22 22 9.27 100.00 204 0.71 - 0.69 22 22 9.64 100.00 212 0.68 - 0.65 27 29 8.89 93.10 240 --------------------------------------------------------------- 7.36 - 0.65 225 227 13.60 99.12 3061 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:48:25 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.375487 7.360217 7.369833 120.1828 120.1035 89.5818 4058 Reflections read from file xs2212a.hkl 4058 Reflections used for space-group determination (up to diffraction limit of 0.46A); mean (I/sigma) = 4.71 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2027 2032 2043 2028 3051 2694 2703 4058 N (int>3sigma) = 0 222 245 331 224 399 625 628 923 Mean intensity = 0.0 0.7 0.7 1.1 0.7 0.8 22.6 23.5 23.3 Mean int/sigma = 0.0 1.4 1.5 1.9 1.4 1.6 4.6 4.8 4.7 Lattice type: P chosen Volume: 282.69 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.360 7.361 119.74 90.19 119.84 Niggli form: a.a = 53.944 b.b = 54.173 c.c = 54.186 b.c = -26.875 a.c = -0.176 a.b = -26.901 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.317 CUBIC F-lattice R(int) = 0.239 [ 3820] Vol = 1130.8 Cell: 10.382 10.458 10.415 90.15 89.87 90.12 Volume: 1130.78 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.316 RHOMBOHEDRAL R-lattice R(int) = 0.219 [ 3386] Vol = 848.1 Cell: 7.360 7.345 18.087 89.83 90.35 119.84 Volume: 848.08 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.316 RHOMBOHEDRAL R-lattice R(int) = 0.226 [ 1097] Vol = 848.1 Trigonal Cell: 7.360 7.345 18.087 89.83 90.35 119.84 Volume: 848.08 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.533 TETRAGONAL I-lattice R(int) = 0.224 [ 3432] Vol = 565.4 Cell: 7.370 7.390 10.382 89.83 89.99 90.23 Volume: 565.39 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.531 TETRAGONAL I-lattice R(int) = 0.224 [ 3432] Vol = 565.4 Cell: 7.370 7.390 10.382 89.83 89.99 90.23 Volume: 565.39 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.369 ORTHORHOMBIC I-lattice R(int) = 0.185 [ 3361] Vol = 565.4 Cell: 7.370 10.382 7.390 89.83 89.77 90.01 Volume: 565.39 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.240 MONOCLINIC I-lattice R(int) = 0.179 [ 2841] Vol = 565.4 Cell: 10.382 7.370 7.390 90.23 90.17 90.01 Volume: 565.39 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.190 MONOCLINIC I-lattice R(int) = 0.176 [ 2830] Vol = 565.4 Cell: 7.361 7.345 10.458 90.03 90.19 89.81 Volume: 565.39 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.249 MONOCLINIC C-lattice R(int) = 0.179 [ 2859] Vol = 565.4 Cell: 10.382 10.458 7.345 90.03 134.84 90.12 Volume: 565.39 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) = 0.122 [ 1880] Vol = 282.7 Cell: 7.345 7.360 7.361 119.74 90.19 119.84 Volume: 282.69 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 2043 0 2703 2693 4058 N (int>3sigma) = 0 0 0 0 331 0 628 633 923 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 23.5 23.6 23.3 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.8 4.8 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.813 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 25 25 297 785 N I>3s 0 0 0 192 0.0 0.0 -0.0 1.4 0.4 0.4 0.1 2.5 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 0.239 3551 Fd-3m 1 1 227 C N N N N 37 2284 0.239 3615 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.381626 10.457679 10.415495 90.1546 89.8718 90.1187 ZERR 1.00 0.005723 0.000945 0.010358 0.0944 0.0037 0.0052 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 823249- 91284 448 431 48 9.0 332595.07 30.43 0.172 0.193 89268- 2456 505 485 48 10.1 12461.63 4.48 0.305 0.179 2356- 1344 739 731 48 15.2 1932.86 2.10 0.861 1.004 1343- 922 585 580 48 12.1 1080.33 1.37 0.754 0.844 910- 715 416 411 48 8.6 812.15 1.18 0.693 0.729 712- 559 435 430 48 9.0 609.85 0.93 0.722 0.848 548- 437 314 311 48 6.5 465.72 0.85 0.645 0.731 437- 283 253 251 48 5.2 366.46 0.75 0.668 0.804 283- 127 265 263 48 5.5 197.89 0.51 0.833 1.193 126- -369 165 165 55 3.0 28.61 0.13 0.983 3.060 ------------------------------------------------------------------------------------------- 823249- -369 4125 4058 487 8.3 37536.10 4.71 0.190 0.204 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-1.14 999 980 48 20.4 77804.20 9.09 0.203 0.236 0.027 1.14-0.89 733 722 49 14.7 39648.90 4.66 0.177 0.180 0.052 0.89-0.76 615 609 49 12.4 32938.93 4.00 0.179 0.222 0.072 0.76-0.69 496 492 50 9.8 23583.56 3.32 0.173 0.209 0.079 0.69-0.63 394 390 48 8.1 18254.36 2.74 0.199 0.212 0.097 0.63-0.59 309 301 49 6.1 9686.62 1.97 0.234 0.228 0.125 0.59-0.55 227 218 48 4.5 14133.29 2.44 0.116 0.110 0.109 0.55-0.52 147 145 48 3.0 5667.14 1.46 0.126 0.122 0.166 0.52-0.49 123 120 48 2.5 12496.67 2.32 0.086 0.092 0.115 0.49-0.45 82 81 50 1.6 4279.99 1.12 0.445 0.520 0.200 ------------------------------------------------------------------------------------------------------ inf-0.45 4125 4058 487 8.3 37536.10 4.71 0.190 0.204 0.050 inf-0.65 3102 3061 225 13.6 45516.14 5.50 0.192 0.218 0.045 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-1.14 980 48 48 100.0 20.4 77804.20 36.66 0.203 0.007 1.14-0.89 722 49 49 100.0 14.7 39648.90 15.54 0.177 0.019 0.89-0.76 609 49 49 100.0 12.4 32938.93 12.98 0.179 0.026 0.76-0.69 492 50 50 100.0 9.8 23583.56 9.93 0.173 0.029 0.69-0.63 390 50 48 96.0 8.1 18254.36 7.72 0.199 0.046 0.63-0.59 301 55 49 89.1 6.1 9686.62 4.68 0.234 0.055 0.59-0.55 218 55 48 87.3 4.5 14133.29 5.28 0.116 0.054 0.55-0.52 145 63 48 76.2 3.0 5667.14 2.54 0.126 0.089 0.52-0.49 120 79 48 60.8 2.5 12496.67 3.69 0.086 0.074 0.49-0.45 81 150 50 33.3 1.6 4279.99 1.41 0.445 0.901 -------------------------------------------------------------------------------------------- inf-0.45 4058 651 487 74.8 8.3 37536.10 16.37 0.190 0.026 inf-0.65 3061 227 225 99.1 13.6 45516.14 20.02 0.192 0.017 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 RRPPROF to HKL transformation matrix: -1.0 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 -2.0 No constraint UB - matrix: -0.066372 0.013075 -0.008900 ( 0.000011 0.000012 0.000012 ) 0.014653 0.065197 -0.013116 ( 0.000010 0.000011 0.000011 ) 0.006120 -0.014602 -0.066265 ( 0.000013 0.000014 0.000014 ) M - matrix: 0.004657 -0.000002 -0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.004635 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000007 -0.000004 0.004642 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.066372 0.013075 -0.008900 ( 0.000011 0.000012 0.000012 ) 0.014653 0.065197 -0.013116 ( 0.000010 0.000011 0.000011 ) 0.006120 -0.014602 -0.066265 ( 0.000013 0.000014 0.000014 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) unit cell: 10.3935(16) 10.4187(19) 10.4103(19) 89.952(15) 89.913(14) 89.977(14) V = 1127.3(3) unit cell: 10.4075(4) 10.4075(4) 10.4075(4) 90.0 90.0 90.0 V = 1127.30(8) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.165) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-565.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-588.7526 max=1114639.8689 PROFFIT INFO: background sum: min=-77.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=394.0000 max=5571.0000 PROFFIT INFO: num of signal pixels: min=41 max=497 PROFFIT INFO: Inet: min=-942.0042 max=1783423.8750 PROFFIT INFO: sig(Inet): min=57.4333 max=24370.4648 PROFFIT INFO: Inet/sig(Inet): min=-1.72 max=198.43 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 730 2916 4334 5178 5544 6434 6964 7298 7832 8160 8250 Percent 8.8 35.3 52.5 62.8 67.2 78.0 84.4 88.5 94.9 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4125 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 4125 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1783424- 126052 412 393286.36 75.92 100.00 124374- 3848 412 29383.98 19.46 100.00 3846- 2012 412 2777.53 6.97 97.33 2012- 1173 412 1535.60 3.79 49.03 1172- 791 412 969.71 2.25 12.62 790- 519 412 651.09 1.68 7.77 519- 319 412 413.93 1.18 4.85 319- 149 412 232.26 0.69 1.21 148- 16 412 78.36 0.29 0.00 15- -942 417 -130.91 -0.26 0.00 ------------------------------------------------------------------------------------ 1783424- -942 4125 42867.61 11.18 37.24 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 412 111432.23 15.12 68.45 1.73- 1.26 412 77447.90 20.83 59.95 1.26- 1.09 412 56878.87 18.27 64.32 1.09- 0.96 412 52594.71 14.74 34.95 0.96- 0.88 412 11921.23 5.78 39.81 0.88- 0.81 412 53327.53 15.10 37.62 0.81- 0.76 412 17767.64 5.60 16.99 0.76- 0.71 412 20870.20 6.87 17.72 0.71- 0.67 412 23233.09 7.80 27.18 0.67- 0.63 417 3678.28 1.83 5.76 ------------------------------------------------------------------------------------ 6.00- 0.63 4125 42867.61 11.18 37.24 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:48:26 2019 Sorting 4125 observations 43 unique observations with > 7.00 F2/sig(F2) 4125 observations in 4 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 103 411 Total number of frames 411 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 4125 observations in 4 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 Total number of frames 44 983 observations > 7.00 F2/sig(F2) 983 observations in 4 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 Total number of frames 44 Removing 'redundancy=1' reflections Average redundancy: 18.9 (Out of 983 removed 1 = 982, unique = 52) 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 982 observations in 4 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 Total number of frames 44 52 unique data precomputed (should be 52) 52 unique data with 982 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 18.9 (Out of 982 removed 0 = 982, unique = 52) 52 unique data precomputed (should be 52) 52 unique data with 982 observations RMS deviation of equivalent data = 0.27649 Rint = 0.19968 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19393, wR= 0.26337 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09501, wR= 0.14596, Acormin=0.576, Acormax=1.378, Acor_av=1.031 F test: Probability=1.000, F= 4.144 Trying model 2 (ne=2, no=1)... Results: Rint= 0.08974, wR= 0.13843, Acormin=0.522, Acormax=1.436, Acor_av=1.003 F test: Probability=0.954, F= 1.117 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08252, wR= 0.13683, Acormin=0.598, Acormax=1.456, Acor_av=1.030 F test: Probability=0.993, F= 1.175 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08030, wR= 0.12526, Acormin=0.527, Acormax=1.572, Acor_av=1.004 F test: Probability=0.780, F= 1.052 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07380, wR= 0.11637, Acormin=0.574, Acormax=1.699, Acor_av=1.014 F test: Probability=0.999, F= 1.236 Final absorption model (ne=4, no=3): Rint= 0.07380, Acormin=0.574, Acormax=1.699, Acor_av=1.014 Combined refinement in use Rint: 0.20181 There are 44 active scales (one needs to be fixed) Refinement control: frame scale #12 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 67 pars with 2278 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.27649 Using Levenberg-Marquardt: 0.00010 New wR= 0.13363 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19968 with corrections 0.09605 Rint for all data: 0.20181 with corrections 0.09870 2 observations identified as outliers and rejected Cycle 2 wR= 0.12571 Using Levenberg-Marquardt: 0.00001 New wR= 0.11560 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19849 with corrections 0.07719 Rint for all data: 0.20181 with corrections 0.08403 3 observations identified as outliers and rejected Cycle 3 wR= 0.09357 Using Levenberg-Marquardt: 0.00000 New wR= 0.07796 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19416 with corrections 0.05690 Rint for all data: 0.20181 with corrections 0.06707 0 observations identified as outliers and rejected Cycle 4 wR= 0.07796 Using Levenberg-Marquardt: 0.00000 New wR= 0.07667 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19416 with corrections 0.05556 Rint for all data: 0.20181 with corrections 0.06575 0 observations identified as outliers and rejected Cycle 5 wR= 0.07667 Using Levenberg-Marquardt: 0.00000 New wR= 0.07611 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19416 with corrections 0.05483 Rint for all data: 0.20181 with corrections 0.06504 0 observations identified as outliers and rejected Final wR= 0.07611 Final frame scales: Min= 0.7855 Max= 1.1330 Final absorption correction factors: Amin= 0.4633 Amax= 1.5210 PROFFIT INFO: Inet (after scale3 abspack): min=-930.8288 max=1218292.6250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=46.5100 max=23744.4199 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/104 4125 reflections read from tmp file 177 reflections are rejected (175 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 3 5 4 5 3 4 3 132 Initial Chi^2= 0.52667 Cycle 1, Chi^2= 1.05538 Current error model SIG(F2)^2 = 72.92*I_RAW + 8.28*I_BACK+(0.02882*)^2 Cycle 2, Chi^2= 1.01748 Current error model SIG(F2)^2 = 84.86*I_RAW + 6.28*I_BACK+(0.02773*)^2 Cycle 3, Chi^2= 1.00365 Current error model SIG(F2)^2 = 87.76*I_RAW + 5.95*I_BACK+(0.02771*)^2 Cycle 4, Chi^2= 1.00077 Current error model SIG(F2)^2 = 88.37*I_RAW + 5.88*I_BACK+(0.02770*)^2 Cycle 5, Chi^2= 1.00016 Current error model SIG(F2)^2 = 88.50*I_RAW + 5.87*I_BACK+(0.02770*)^2 Final Chi^2= 1.00016 Final error model SIG(F2)^2 = 88.50*I_RAW + 5.87*I_BACK+(0.02770*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1218293- 116849 412 377402.55 29.72 100.00 115323- 3465 412 29451.47 12.67 100.00 3450- 1986 412 2647.23 5.91 99.27 1985- 1136 412 1497.09 3.86 64.08 1135- 765 412 924.85 2.63 19.17 765- 510 412 629.79 2.25 11.89 509- 311 412 405.90 1.92 9.71 311- 146 412 227.47 1.36 1.94 146- 15 412 78.65 0.70 0.00 15- -931 417 -128.33 -0.55 0.00 ------------------------------------------------------------------------------------ 1218293- -931 4125 41263.43 6.04 40.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 412 107737.37 9.90 71.36 1.73- 1.26 412 76151.68 8.97 62.38 1.26- 1.09 412 55979.04 7.88 68.45 1.09- 0.96 412 49471.91 6.50 37.62 0.96- 0.88 412 12019.32 4.18 46.36 0.88- 0.81 412 50490.26 7.75 42.23 0.81- 0.76 412 16633.55 3.62 19.17 0.76- 0.71 412 19132.98 4.70 19.90 0.71- 0.67 412 21891.06 5.21 31.55 0.67- 0.63 417 3584.43 1.71 6.95 ------------------------------------------------------------------------------------ 6.00- 0.63 4125 41263.43 6.04 40.56 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 412 107737.37 9.90 71.36 6.00- 1.26 824 91944.52 9.44 66.87 6.00- 1.09 1236 79956.03 8.92 67.39 6.00- 0.96 1648 72335.00 8.31 59.95 6.00- 0.88 2060 60271.86 7.49 57.23 6.00- 0.81 2472 58641.60 7.53 54.73 6.00- 0.76 2884 52640.45 6.97 49.65 6.00- 0.71 3296 48452.01 6.69 45.93 6.00- 0.67 3708 45500.80 6.52 44.34 6.00- 0.63 4125 41263.43 6.04 40.56 ------------------------------------------------------------------------------------ 6.00- 0.63 4125 41263.43 6.04 40.56 Scale applied to data: s=0.820820 (maximum obs:1218292.625,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.065; Rsigma 0.039: data 4125 -> merged 162 With outlier rejection... Rint 0.054; Rsigma 0.039: data 4106 -> merged 162 Rejected total: 19, method kkm 13, method Blessing 6 Completeness direct cell (a, b, c) = (10.407, 10.407, 10.407), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626457, 6.008767 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.76 14 14 27.07 100.00 379 1.73 - 1.27 14 14 29.64 100.00 415 1.26 - 1.06 14 14 33.50 100.00 469 1.05 - 0.97 14 14 29.00 100.00 406 0.95 - 0.88 14 14 30.29 100.00 424 0.87 - 0.81 14 14 26.86 100.00 376 0.80 - 0.76 14 14 28.43 100.00 398 0.76 - 0.72 14 14 23.71 100.00 332 0.72 - 0.69 14 14 25.71 100.00 360 0.69 - 0.65 19 19 21.84 100.00 415 --------------------------------------------------------------- 7.36 - 0.65 145 145 27.41 100.00 3974 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:48:25 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.375487 7.360217 7.369833 120.1828 120.1035 89.5818 4058 Reflections read from file xs2212a.hkl 4058 Reflections used for space-group determination (up to diffraction limit of 0.46A); mean (I/sigma) = 4.71 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2027 2032 2043 2028 3051 2694 2703 4058 N (int>3sigma) = 0 222 245 331 224 399 625 628 923 Mean intensity = 0.0 0.7 0.7 1.1 0.7 0.8 22.6 23.5 23.3 Mean int/sigma = 0.0 1.4 1.5 1.9 1.4 1.6 4.6 4.8 4.7 Lattice type: P chosen Volume: 282.69 ------------------------------------------------------------------------------- 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 0.0000 1.0000 Unitcell: 7.345 7.360 7.361 119.74 90.19 119.84 Niggli form: a.a = 53.944 b.b = 54.173 c.c = 54.186 b.c = -26.875 a.c = -0.176 a.b = -26.901 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.317 CUBIC F-lattice R(int) = 0.239 [ 3820] Vol = 1130.8 Cell: 10.382 10.458 10.415 90.15 89.87 90.12 Volume: 1130.78 Matrix:-1.0000 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.316 RHOMBOHEDRAL R-lattice R(int) = 0.219 [ 3386] Vol = 848.1 Cell: 7.360 7.345 18.087 89.83 90.35 119.84 Volume: 848.08 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.316 RHOMBOHEDRAL R-lattice R(int) = 0.226 [ 1097] Vol = 848.1 Trigonal Cell: 7.360 7.345 18.087 89.83 90.35 119.84 Volume: 848.08 Matrix: 0.0000 1.0000 0.0000 0.0000 -1.0000 -1.0000 -3.0000 -1.0000 -2.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.533 TETRAGONAL I-lattice R(int) = 0.224 [ 3432] Vol = 565.4 Cell: 7.370 7.390 10.382 89.83 89.99 90.23 Volume: 565.39 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.531 TETRAGONAL I-lattice R(int) = 0.224 [ 3432] Vol = 565.4 Cell: 7.370 7.390 10.382 89.83 89.99 90.23 Volume: 565.39 Matrix: 0.0000 0.0000 -1.0000 -1.0000 -1.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.369 ORTHORHOMBIC I-lattice R(int) = 0.185 [ 3361] Vol = 565.4 Cell: 7.370 10.382 7.390 89.83 89.77 90.01 Volume: 565.39 Matrix: 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.240 MONOCLINIC I-lattice R(int) = 0.179 [ 2841] Vol = 565.4 Cell: 10.382 7.370 7.390 90.23 90.17 90.01 Volume: 565.39 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.190 MONOCLINIC I-lattice R(int) = 0.176 [ 2830] Vol = 565.4 Cell: 7.361 7.345 10.458 90.03 90.19 89.81 Volume: 565.39 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.249 MONOCLINIC C-lattice R(int) = 0.179 [ 2859] Vol = 565.4 Cell: 10.382 10.458 7.345 90.03 134.84 90.12 Volume: 565.39 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) = 0.122 [ 1880] Vol = 282.7 Cell: 7.345 7.360 7.361 119.74 90.19 119.84 Volume: 282.69 Matrix: 0.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 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 2043 0 2703 2693 4058 N (int>3sigma) = 0 0 0 0 331 0 628 633 923 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 23.5 23.6 23.3 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.8 4.8 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.813 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 25 25 297 785 N I>3s 0 0 0 192 0.0 0.0 -0.0 1.4 0.4 0.4 0.1 2.5 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 0.239 3551 Fd-3m 1 1 227 C N N N N 37 2284 0.239 3615 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.381626 10.457679 10.415495 90.1546 89.8718 90.1187 ZERR 1.00 0.005723 0.000945 0.010358 0.0944 0.0037 0.0052 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1126970- 93795 505 494 27 18.3 326036.88 27.87 0.050 0.061 74927- 1663 832 827 27 30.6 4911.34 7.80 0.096 0.115 1659- 757 758 756 27 28.0 1067.02 2.72 0.246 0.305 702- 321 814 814 27 30.1 487.29 1.89 0.386 0.545 313- 63 606 605 27 22.4 214.94 1.14 0.600 0.941 63- -160 610 610 27 22.6 8.63 0.17 0.957 3.886 ------------------------------------------------------------------------------------------- 1126970- -160 4125 4106 162 25.3 40541.29 5.99 0.054 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-1.27 798 792 27 29.3 91890.63 9.58 0.044 0.051 0.031 1.26-0.97 878 875 28 31.3 49245.30 6.80 0.051 0.068 0.035 0.95-0.81 802 800 28 28.6 32132.13 6.10 0.058 0.071 0.044 0.80-0.73 712 711 27 26.3 17036.09 4.01 0.078 0.096 0.057 0.72-0.67 626 625 27 23.1 18513.28 4.50 0.087 0.113 0.064 0.66-0.63 309 303 25 12.1 3981.31 1.77 0.111 0.080 0.126 ------------------------------------------------------------------------------------------------------ inf-0.63 4125 4106 162 25.3 40541.29 5.99 0.054 0.065 0.039 inf-0.65 3986 3972 144 27.6 41673.67 6.12 0.054 0.064 0.039 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-1.27 792 27 27 100.0 29.3 91890.63 50.24 0.044 0.008 1.26-0.97 875 28 28 100.0 31.3 49245.30 36.14 0.051 0.008 0.95-0.81 800 28 28 100.0 28.6 32132.13 33.08 0.058 0.010 0.80-0.73 711 27 27 100.0 26.3 17036.09 18.81 0.078 0.013 0.72-0.67 625 27 27 100.0 23.1 18513.28 23.52 0.087 0.014 0.66-0.63 303 25 25 100.0 12.1 3981.31 6.63 0.111 0.040 -------------------------------------------------------------------------------------------- inf-0.63 4106 162 162 100.0 25.3 40541.29 31.17 0.054 0.010 inf-0.65 3972 144 144 100.0 27.6 41673.67 32.03 0.054 0.009 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 13:54:59 2019) ID: 3668; threads 40; handles 809; mem 515868.00 (1204688.00)kB; time: 1w 5d 0h 5m 47s MEMORY INFO: Memory PF:228.0, Ph:557.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:503.8,peak PF: 700.2, WS: 471.5, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:230.0, Ph:559.0, V:1178.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:505.6,peak PF: 700.2, WS: 473.3, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 13:54:59 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000084 0.000065 0.000085 ) 0.064809 0.092374 0.027273 ( 0.000100 0.000078 0.000101 ) 0.045523 0.057900 0.132205 ( 0.000121 0.000093 0.000122 ) 7.38096 ( 0.00662 ) 7.36649 ( 0.00716 ) 7.42630 ( 0.00818 ) 120.52449 ( 0.11056 ) 120.40327 ( 0.10624 ) 89.27095 ( 0.07567 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 13:54:59 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000084 0.000065 0.000085 ) 0.064809 0.092374 0.027273 ( 0.000100 0.000078 0.000101 ) 0.045523 0.057900 0.132205 ( 0.000121 0.000093 0.000122 ) M - matrix: 0.013767 0.004514 0.009162 ( 0.000022 0.000015 0.000020 ) 0.004514 0.013970 0.009339 ( 0.000015 0.000019 0.000018 ) 0.009162 0.009339 0.018547 ( 0.000020 0.000018 0.000033 ) unit cell: 7.381(7) 7.366(7) 7.426(8) 120.52(11) 120.40(11) 89.27(8) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.82 | 24 | 1.005 ( 0.047) | 1.008 ( 0.130) | 0.907 ( 0.354) | 0.79- 0.69 | 24 | 0.998 ( 0.044) | 1.006 ( 0.137) | 1.289 ( 0.497) | 0.69- 0.63 | 23 | 0.979 ( 0.051) | 0.913 ( 0.103) | 1.157 ( 0.432) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.510) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 46 obs out of 238 (total:238,skipped:0) (19.33%) UB - matrix: 0.086322 -0.045974 0.017116 ( 0.000473 0.000165 0.000229 ) 0.064318 0.092941 0.027760 ( 0.000633 0.000220 0.000306 ) 0.045617 0.058321 0.132889 ( 0.000830 0.000289 0.000401 ) M - matrix: 0.013669 0.004670 0.009325 ( 0.000138 0.000083 0.000117 ) 0.004670 0.014153 0.009543 ( 0.000083 0.000055 0.000055 ) 0.009325 0.009543 0.018723 ( 0.000117 0.000055 0.000108 ) unit cell: 7.47(3) 7.36(3) 7.42(3) 120.7(5) 120.4(5) 89.5(4) V = 285(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 4, #refl in peak table: 238 #indexed refl 216, indexation with best UB: 90.7563% Lattice: 7.4072 7.3556 7.3610 120.005 120.354 89.764 282.632 Rotation: -22.660 24.759 -35.022 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 227 obs out of 238 (total:238,skipped:0) (95.38%) UB - matrix: 0.087760 -0.044390 0.012681 ( 0.000052 0.000055 0.000059 ) 0.061495 0.094382 0.026268 ( 0.000060 0.000065 0.000069 ) 0.049386 0.055440 0.133261 ( 0.000059 0.000063 0.000067 ) M - matrix: 0.013922 0.004646 0.009310 ( 0.000013 0.000010 0.000011 ) 0.004646 0.013952 0.009304 ( 0.000010 0.000015 0.000012 ) 0.009310 0.009304 0.018609 ( 0.000011 0.000012 0.000018 ) unit cell: 7.369(4) 7.355(5) 7.360(5) 120.01(7) 120.09(6) 89.95(5) V = 281.8(3) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1316 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 223 peaks identified as outliers and rejected 223 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 223 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 223 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 2.38 | 22 | 0.899 ( 0.094) | 0.905 ( 0.131) | 0.958 ( 0.493) | 2.38- 1.83 | 22 | 0.900 ( 0.110) | 0.921 ( 0.154) | 0.939 ( 0.269) | 1.76- 1.58 | 22 | 0.887 ( 0.115) | 0.904 ( 0.161) | 0.806 ( 0.264) | 1.58- 1.35 | 22 | 0.954 ( 0.082) | 0.983 ( 0.130) | 0.791 ( 0.395) | 1.35- 1.19 | 22 | 0.935 ( 0.082) | 0.954 ( 0.100) | 0.903 ( 0.428) | 1.19- 1.00 | 22 | 0.962 ( 0.087) | 0.981 ( 0.123) | 0.884 ( 0.304) | 1.00- 0.88 | 22 | 0.988 ( 0.064) | 0.995 ( 0.081) | 1.052 ( 0.398) | 0.88- 0.79 | 22 | 0.993 ( 0.048) | 0.994 ( 0.129) | 0.938 ( 0.310) | 0.79- 0.69 | 22 | 0.975 ( 0.044) | 0.932 ( 0.088) | 1.196 ( 0.465) | 0.69- 0.63 | 25 | 0.933 ( 0.047) | 0.852 ( 0.068) | 1.275 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 0.63 | 223 | 0.942 ( 0.089) | 0.941 ( 0.128) | 0.978 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) UB - matrix: 0.088106 -0.044293 0.012828 ( 0.000028 0.000032 0.000033 ) 0.061394 0.094519 0.026063 ( 0.000022 0.000026 0.000027 ) 0.049283 0.055378 0.133130 ( 0.000021 0.000024 0.000025 ) M - matrix: 0.013961 0.004630 0.009291 ( 0.000006 0.000004 0.000005 ) 0.004630 0.013962 0.009268 ( 0.000004 0.000006 0.000005 ) 0.009291 0.009268 0.018567 ( 0.000005 0.000005 0.000007 ) unit cell: 7.351(2) 7.341(2) 7.3536(18) 119.91(3) 120.04(3) 89.95(2) V = 280.88(13) OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 UB - matrix: 0.087896 -0.044356 0.012683 ( 0.000021 0.000024 0.000025 ) 0.061495 0.094417 0.026185 ( 0.000020 0.000022 0.000024 ) 0.049387 0.055447 0.133218 ( 0.000019 0.000022 0.000023 ) M - matrix: 0.013946 0.004646 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013956 0.009296 ( 0.000004 0.000005 0.000004 ) 0.009304 0.009296 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3589(17) 7.3517(18) 7.3584(16) 119.99(2) 120.05(2) 89.96(2) V = 281.42(11) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087896 -0.044356 0.012683 ( 0.000021 0.000024 0.000025 ) 0.061495 0.094417 0.026185 ( 0.000020 0.000022 0.000024 ) 0.049387 0.055447 0.133218 ( 0.000019 0.000022 0.000023 ) M - matrix: 0.013946 0.004646 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013956 0.009296 ( 0.000004 0.000005 0.000004 ) 0.009304 0.009296 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3589(17) 7.3517(18) 7.3584(16) 119.99(2) 120.05(2) 89.96(2) V = 281.42(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) 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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 223 peaks identified as outliers and rejected 223 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 223 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 223 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 22 | 0.868 ( 0.103) | 0.880 ( 0.128) | 0.911 ( 0.399) | 2.38- 1.83 | 22 | 0.907 ( 0.104) | 0.924 ( 0.157) | 0.918 ( 0.259) | 1.76- 1.59 | 22 | 0.880 ( 0.117) | 0.891 ( 0.164) | 0.729 ( 0.225) | 1.58- 1.45 | 22 | 0.947 ( 0.083) | 0.969 ( 0.129) | 0.883 ( 0.461) | 1.45- 1.19 | 22 | 0.926 ( 0.075) | 0.944 ( 0.084) | 0.839 ( 0.422) | 1.19- 1.06 | 22 | 0.980 ( 0.083) | 1.000 ( 0.124) | 0.894 ( 0.363) | 1.01- 0.88 | 22 | 0.983 ( 0.064) | 1.014 ( 0.078) | 1.039 ( 0.371) | 0.88- 0.79 | 22 | 0.991 ( 0.048) | 0.987 ( 0.128) | 0.966 ( 0.330) | 0.79- 0.69 | 22 | 0.976 ( 0.044) | 0.935 ( 0.090) | 1.283 ( 0.490) | 0.69- 0.63 | 25 | 0.933 ( 0.048) | 0.854 ( 0.073) | 1.273 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 223 | 0.939 ( 0.090) | 0.939 ( 0.130) | 0.977 ( 0.421) | 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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb PROFFITPEAK info: 90 peaks in the peak location table UB fit with 9 obs out of 55 (total:55,skipped:0) (16.36%) UB - matrix: 0.086573 -0.050141 0.015680 ( 0.001026 0.003269 0.001426 ) 0.063445 0.088932 0.025700 ( 0.000764 0.002435 0.001062 ) 0.044696 0.055837 0.131260 ( 0.000537 0.001711 0.000746 ) M - matrix: 0.013518 0.003797 0.008855 ( 0.000208 0.000343 0.000163 ) 0.003797 0.013541 0.008829 ( 0.000343 0.000576 0.000270 ) 0.008855 0.008829 0.018135 ( 0.000163 0.000270 0.000208 ) unit cell: 7.41(16) 7.39(17) 7.43(9) 121(2) 121(2) 87(2) V = 288(9) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 5, #refl in peak table: 55 #indexed refl 50, indexation with best UB: 90.9091% Lattice: 7.3744 7.3165 7.3417 119.879 120.427 89.210 280.691 Rotation: -22.532 24.695 -35.038 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 54 obs out of 55 (total:55,skipped:0) (98.18%) UB - matrix: 0.087864 -0.044505 0.012469 ( 0.000069 0.000229 0.000081 ) 0.061512 0.094729 0.026097 ( 0.000086 0.000285 0.000100 ) 0.049267 0.055247 0.133189 ( 0.000054 0.000180 0.000063 ) M - matrix: 0.013931 0.004638 0.009263 ( 0.000017 0.000030 0.000012 ) 0.004638 0.014007 0.009276 ( 0.000030 0.000061 0.000027 ) 0.009263 0.009276 0.018576 ( 0.000012 0.000027 0.000018 ) unit cell: 7.350(12) 7.326(16) 7.339(9) 119.85(18) 119.91(15) 90.08(16) V = 280.2(8) OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 UB - matrix: 0.087986 -0.044455 0.012565 ( 0.000066 0.000221 0.000078 ) 0.061526 0.094783 0.026188 ( 0.000086 0.000285 0.000100 ) 0.049213 0.055212 0.133129 ( 0.000054 0.000180 0.000064 ) M - matrix: 0.013949 0.004637 0.009269 ( 0.000017 0.000029 0.000012 ) 0.004637 0.014008 0.009274 ( 0.000029 0.000061 0.000027 ) 0.009269 0.009274 0.018567 ( 0.000012 0.000027 0.000018 ) UB fit with 54 obs out of 55 (total:55,skipped:0) (98.18%) unit cell: 7.346(12) 7.325(16) 7.342(9) 119.86(18) 119.94(15) 90.05(15) V = 280.1(8) UB fit with 54 obs out of 55 (total:55,skipped:0) (98.18%) UB - matrix: 0.087986 -0.044455 0.012565 ( 0.000066 0.000221 0.000078 ) 0.061526 0.094783 0.026188 ( 0.000086 0.000285 0.000100 ) 0.049213 0.055212 0.133129 ( 0.000054 0.000180 0.000064 ) M - matrix: 0.013949 0.004637 0.009269 ( 0.000017 0.000029 0.000012 ) 0.004637 0.014008 0.009274 ( 0.000029 0.000061 0.000027 ) 0.009269 0.009274 0.018567 ( 0.000012 0.000027 0.000018 ) unit cell: 7.346(12) 7.325(16) 7.342(9) 119.86(18) 119.94(15) 90.05(15) V = 280.1(8) 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 55 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Run 5 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 457 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 54 obs out of 55 (total:55,skipped:0) (98.18%) 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= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb 0 of 50 peaks identified as outliers and rejected 50 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 50 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 50 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.35 | 5 | 0.851 ( 0.095) | 0.844 ( 0.115) | 0.972 ( 0.257) | 2.12- 1.83 | 5 | 0.933 ( 0.119) | 0.958 ( 0.146) | 0.760 ( 0.187) | 1.75- 1.57 | 5 | 0.976 ( 0.108) | 0.954 ( 0.110) | 1.013 ( 0.476) | 1.57- 1.45 | 5 | 0.990 ( 0.095) | 0.996 ( 0.119) | 0.650 ( 0.179) | 1.35- 1.22 | 5 | 0.949 ( 0.096) | 0.959 ( 0.156) | 0.688 ( 0.204) | 1.22- 1.11 | 5 | 0.978 ( 0.034) | 0.947 ( 0.078) | 0.981 ( 0.347) | 1.10- 1.00 | 5 | 0.959 ( 0.072) | 0.953 ( 0.101) | 0.807 ( 0.280) | 1.00- 0.87 | 5 | 1.007 ( 0.091) | 1.022 ( 0.058) | 0.873 ( 0.266) | 0.82- 0.75 | 5 | 1.037 ( 0.033) | 1.065 ( 0.132) | 0.961 ( 0.365) | 0.73- 0.67 | 5 | 1.007 ( 0.039) | 1.025 ( 0.136) | 1.188 ( 0.436) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.67 | 50 | 0.969 ( 0.097) | 0.972 ( 0.132) | 0.889 ( 0.352) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) UB - matrix: 0.088147 -0.044654 0.012787 ( 0.000041 0.000158 0.000049 ) 0.061708 0.094869 0.026455 ( 0.000056 0.000215 0.000066 ) 0.049326 0.055176 0.133180 ( 0.000029 0.000112 0.000034 ) M - matrix: 0.014011 0.004640 0.009329 ( 0.000010 0.000021 0.000007 ) 0.004640 0.014038 0.009287 ( 0.000021 0.000045 0.000017 ) 0.009329 0.009287 0.018600 ( 0.000007 0.000017 0.000010 ) unit cell: 7.343(8) 7.315(12) 7.349(6) 119.87(12) 120.14(10) 89.89(11) V = 279.4(6) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: 0.087818 -0.044727 0.012512 ( 0.000029 0.000112 0.000035 ) 0.061644 0.094819 0.026257 ( 0.000042 0.000161 0.000049 ) 0.049309 0.055125 0.133163 ( 0.000026 0.000102 0.000031 ) M - matrix: 0.013944 0.004635 0.009284 ( 0.000008 0.000015 0.000006 ) 0.004635 0.014030 0.009271 ( 0.000015 0.000034 0.000015 ) 0.009284 0.009271 0.018578 ( 0.000006 0.000015 0.000009 ) UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) unit cell: 7.353(6) 7.314(9) 7.341(5) 119.80(10) 120.02(8) 90.02(8) V = 279.9(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 456 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb 0 of 50 peaks identified as outliers and rejected 50 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 50 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 50 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.12- 2.37 | 5 | 0.857 ( 0.104) | 0.886 ( 0.172) | 0.866 ( 0.078) | 2.12- 1.84 | 5 | 0.931 ( 0.120) | 0.954 ( 0.151) | 0.713 ( 0.164) | 1.76- 1.56 | 5 | 0.958 ( 0.102) | 0.969 ( 0.120) | 0.956 ( 0.519) | 1.56- 1.35 | 5 | 1.008 ( 0.098) | 1.002 ( 0.124) | 0.728 ( 0.203) | 1.35- 1.22 | 5 | 0.945 ( 0.079) | 0.965 ( 0.156) | 0.696 ( 0.195) | 1.20- 1.11 | 5 | 0.982 ( 0.033) | 0.937 ( 0.065) | 0.935 ( 0.360) | 1.06- 1.00 | 5 | 1.005 ( 0.096) | 0.992 ( 0.125) | 0.803 ( 0.268) | 1.00- 0.87 | 5 | 0.979 ( 0.072) | 0.961 ( 0.031) | 1.116 ( 0.232) | 0.82- 0.75 | 5 | 1.037 ( 0.033) | 1.067 ( 0.136) | 0.964 ( 0.367) | 0.73- 0.67 | 5 | 1.007 ( 0.040) | 1.027 ( 0.138) | 1.187 ( 0.436) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.12- 0.67 | 50 | 0.971 ( 0.097) | 0.976 ( 0.137) | 0.896 ( 0.349) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 98 | 0.985 ( 0.037) | 1.029 ( 0.068) | 1.116 ( 0.485) | 10.3-14.9 | 98 | 0.986 ( 0.045) | 1.040 ( 0.068) | 1.154 ( 0.530) | 14.9-18.9 | 98 | 0.995 ( 0.214) | 1.022 ( 0.098) | 1.187 ( 1.106) | 19.0-23.6 | 98 | 0.960 ( 0.057) | 1.002 ( 0.079) | 0.927 ( 0.414) | 23.6-27.4 | 98 | 0.961 ( 0.063) | 0.992 ( 0.092) | 0.939 ( 0.424) | 27.5-32.6 | 98 | 0.949 ( 0.084) | 0.961 ( 0.114) | 0.933 ( 0.433) | 32.6-36.4 | 98 | 0.917 ( 0.161) | 0.895 ( 0.131) | 1.066 ( 0.649) | 36.4-39.0 | 98 | 0.881 ( 0.094) | 0.852 ( 0.131) | 1.010 ( 0.496) | 39.0-42.0 | 98 | 0.899 ( 0.091) | 0.848 ( 0.125) | 1.056 ( 0.469) | 42.0-50.1 | 96 | 0.868 ( 0.118) | 0.792 ( 0.134) | 0.929 ( 0.459) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 978 | 0.940 ( 0.118) | 0.944 ( 0.136) | 1.032 ( 0.589) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.14 e2 dimension: a=-0.0070 b=1.24 e3 dimension: a=0.0015 b=1.06 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3814 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1336989 PROFFITPEAK - Finished at Wed Aug 21 13:55:12 2019 PROFFITMAIN - Started at Wed Aug 21 13:55:12 2019 OTKP changes: 359 2 4 5 OTKP changes: 359 2 4 5 OTKP changes: 359 2 4 5 UB - matrix: 0.087751 -0.046009 0.016731 ( 0.000079 0.000064 0.000080 ) 0.063096 0.092345 0.026730 ( 0.000090 0.000073 0.000092 ) 0.045325 0.057583 0.131928 ( 0.000095 0.000077 0.000097 ) M - matrix: 0.013736 0.004399 0.009134 ( 0.000020 0.000013 0.000016 ) 0.004399 0.013960 0.009295 ( 0.000013 0.000017 0.000015 ) 0.009134 0.009295 0.018399 ( 0.000016 0.000015 0.000026 ) UB fit with 420 obs out of 978 (total:978,skipped:0) (42.94%) unit cell: 7.397(6) 7.371(7) 7.439(7) 120.81(10) 120.35(9) 88.66(7) V = 285.0(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 197 obs out of 212 (total:212,skipped:0) (92.92%) UB - matrix: 0.087686 -0.046159 0.017190 ( 0.000107 0.000066 0.000100 ) 0.064444 0.092328 0.027075 ( 0.000093 0.000057 0.000087 ) 0.045668 0.057714 0.132017 ( 0.000115 0.000071 0.000107 ) M - matrix: 0.013927 0.004538 0.009281 ( 0.000025 0.000014 0.000019 ) 0.004538 0.013986 0.009326 ( 0.000014 0.000015 0.000015 ) 0.009281 0.009326 0.018457 ( 0.000019 0.000015 0.000029 ) unit cell: 7.372(7) 7.366(7) 7.436(7) 120.57(10) 120.44(10) 89.06(7) V = 283.5(5) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.172) HKL list info: 1291 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087478 -0.046191 0.017344 ( 0.000100 0.000062 0.000093 ) 0.064786 0.092362 0.027264 ( 0.000086 0.000053 0.000080 ) 0.045677 0.057801 0.132104 ( 0.000104 0.000065 0.000097 ) M - matrix: 0.013936 0.004583 0.009318 ( 0.000023 0.000013 0.000018 ) 0.004583 0.014005 0.009353 ( 0.000013 0.000014 0.000013 ) 0.009318 0.009353 0.018496 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.379(7) 7.365(6) 7.435(6) 120.52(9) 120.46(9) 89.20(7) V = 283.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 204 obs out of 212 (total:212,skipped:0) (96.23%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.117984 0.038986 0.078609 ( 0.000076 0.000047 0.000070 ) 0.000087 0.111545 0.056284 ( 0.000080 0.000050 0.000074 ) -0.000023 -0.000076 0.095368 ( 0.000090 0.000056 0.000083 ) M - matrix: 0.013920 0.004609 0.009277 ( 0.000018 0.000011 0.000014 ) 0.004609 0.013962 0.009336 ( 0.000011 0.000012 0.000011 ) 0.009277 0.009336 0.018442 ( 0.000014 0.000011 0.000021 ) UB fit with 206 obs out of 212 (total:212,skipped:0) (97.17%) unit cell: 7.374(5) 7.381(5) 7.434(8) 120.48(9) 120.25(9) 89.46(6) V = 284.2(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.087804 -0.044309 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094149 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055798 0.133161 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004658 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009312 0.018585 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3551(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) UB - matrix: 0.087903 -0.044369 0.012678 ( 0.000021 0.000024 0.000026 ) 0.061483 0.094414 0.026172 ( 0.000019 0.000022 0.000023 ) 0.049390 0.055433 0.133214 ( 0.000017 0.000020 0.000021 ) M - matrix: 0.013947 0.004643 0.009303 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013955 0.009293 ( 0.000004 0.000005 0.000004 ) 0.009303 0.009293 0.018592 ( 0.000004 0.000004 0.000006 ) unit cell: 7.3585(17) 7.3510(18) 7.3581(15) 119.98(2) 120.05(2) 89.95(2) V = 281.39(11) OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1296 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087903 -0.044369 0.012678 ( 0.000021 0.000024 0.000026 ) 0.061483 0.094414 0.026172 ( 0.000019 0.000022 0.000023 ) 0.049390 0.055433 0.133214 ( 0.000017 0.000020 0.000021 ) M - matrix: 0.013947 0.004643 0.009303 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013955 0.009293 ( 0.000004 0.000005 0.000004 ) 0.009303 0.009293 0.018592 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3585(17) 7.3510(18) 7.3581(15) 119.98(2) 120.05(2) 89.95(2) V = 281.39(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* UB - matrix: 0.118100 0.039327 0.078777 ( 0.000021 0.000024 0.000026 ) 0.000003 0.111393 0.055619 ( 0.000011 0.000012 0.000013 ) -0.000002 0.000003 0.096401 ( 0.000023 0.000027 0.000029 ) M - matrix: 0.013948 0.004645 0.009304 ( 0.000005 0.000003 0.000004 ) 0.004645 0.013955 0.009294 ( 0.000003 0.000003 0.000004 ) 0.009304 0.009294 0.018592 ( 0.000004 0.000004 0.000007 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3582(16) 7.3514(13) 7.358(3) 119.98(3) 120.05(3) 89.965(17) V = 281.39(12) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) UB - matrix: 0.087813 -0.044765 0.012513 ( 0.000027 0.000107 0.000034 ) 0.061645 0.094873 0.026290 ( 0.000040 0.000157 0.000049 ) 0.049317 0.055179 0.133167 ( 0.000025 0.000097 0.000030 ) M - matrix: 0.013943 0.004639 0.009287 ( 0.000007 0.000015 0.000006 ) 0.004639 0.014050 0.009282 ( 0.000015 0.000033 0.000015 ) 0.009287 0.009282 0.018581 ( 0.000006 0.000015 0.000009 ) unit cell: 7.354(6) 7.311(9) 7.343(5) 119.82(9) 120.04(8) 90.00(8) V = 279.8(4) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: 0.087782 -0.044772 0.012486 ( 0.000028 0.000110 0.000034 ) 0.061639 0.094870 0.026272 ( 0.000040 0.000154 0.000048 ) 0.049312 0.055173 0.133162 ( 0.000025 0.000096 0.000030 ) M - matrix: 0.013937 0.004638 0.009282 ( 0.000007 0.000015 0.000006 ) 0.004638 0.014049 0.009280 ( 0.000015 0.000033 0.000014 ) 0.009282 0.009280 0.018578 ( 0.000006 0.000014 0.000008 ) UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) unit cell: 7.355(6) 7.311(8) 7.343(5) 119.82(9) 120.03(8) 90.01(8) V = 279.8(4) Run 5 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 433 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* UB - matrix: 0.087782 -0.044772 0.012486 ( 0.000028 0.000110 0.000034 ) 0.061639 0.094870 0.026272 ( 0.000040 0.000154 0.000048 ) 0.049312 0.055173 0.133162 ( 0.000025 0.000096 0.000030 ) M - matrix: 0.013937 0.004638 0.009282 ( 0.000007 0.000015 0.000006 ) 0.004638 0.014049 0.009280 ( 0.000015 0.000033 0.000014 ) 0.009282 0.009280 0.018578 ( 0.000006 0.000014 0.000008 ) UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) unit cell: 7.355(6) 7.311(8) 7.343(5) 119.82(9) 120.03(8) 90.01(8) V = 279.8(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 69.89 ph= 92.09 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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117626 0.038575 0.078505 ( 0.000040 0.000039 0.000045 ) -0.000008 0.111487 0.056115 ( 0.000026 0.000026 0.000029 ) -0.000047 -0.000125 0.096158 ( 0.000027 0.000026 0.000030 ) M - matrix: 0.013836 0.004537 0.009229 ( 0.000009 0.000006 0.000007 ) 0.004537 0.013917 0.009272 ( 0.000006 0.000006 0.000006 ) 0.009229 0.009272 0.018558 ( 0.000007 0.000006 0.000010 ) UB fit with 971 obs out of 978 (total:978,skipped:0) (99.28%) unit cell: 7.377(3) 7.361(2) 7.370(3) 120.20(3) 120.12(4) 89.54(3) V = 282.73(16) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 92 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof 4368 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 13:55:20 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.172) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) Run 5 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-565.0000 max=7905880.0000 PROFFIT INFO: signal sum lp corr: min=-667.9608 max=1115295.6875 PROFFIT INFO: background sum: min=-77.0000 max=7581.0000 PROFFIT INFO: background sum sig2: min=394.0000 max=5651.0000 PROFFIT INFO: num of signal pixels: min=41 max=501 PROFFIT INFO: Inet: min=-1068.7372 max=1784473.0000 PROFFIT INFO: sig(Inet): min=49.1396 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.72 max=198.55 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 384 1532 2285 2734 2928 3406 3688 3865 4149 4321 4368 Percent 8.8 35.1 52.3 62.6 67.0 78.0 84.4 88.5 95.0 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4368 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 4368 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1784473- 127526 436 391871.80 75.79 100.00 126474- 3839 436 29247.40 19.51 100.00 3832- 2038 436 2786.04 7.02 97.94 2033- 1193 436 1555.23 3.84 50.46 1191- 797 436 977.34 2.26 12.61 795- 529 436 658.53 1.66 7.11 529- 327 436 423.71 1.25 5.73 327- 154 436 240.10 0.69 0.92 154- 17 436 81.69 0.29 0.00 16- -1069 444 -126.40 -0.25 0.00 ------------------------------------------------------------------------------------ 1784473- -1069 4368 42692.98 11.18 37.41 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 436 93066.06 15.93 69.50 1.75- 1.28 436 98035.35 22.22 59.40 1.28- 1.06 436 43610.70 13.04 48.62 1.06- 0.92 436 35850.29 11.45 40.14 0.92- 0.83 436 38672.91 11.46 33.49 0.83- 0.75 436 34230.29 10.58 35.09 0.75- 0.69 436 30144.56 9.43 30.05 0.69- 0.63 436 21900.16 7.00 23.62 0.63- 0.57 436 15888.27 5.47 18.12 0.57- 0.44 444 16020.59 5.37 16.44 ------------------------------------------------------------------------------------ 6.55- 0.44 4368 42692.98 11.18 37.41 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:55:20 2019 Sorting 4368 observations 85 unique observations with > 7.00 F2/sig(F2) 4368 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 103 411 5 0 24 436 Total number of frames 436 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 4368 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 17 36 3 0 16 53 4 0 17 71 5 0 4 76 Total number of frames 76 1042 observations > 7.00 F2/sig(F2) 1042 observations in 5 runs Run # start # end # total # 1 0 16 17 2 0 16 34 3 0 16 51 4 0 17 69 5 0 3 73 Total number of frames 73 Removing 'redundancy=1' reflections Average redundancy: 7.8 (Out of 1042 removed 28 = 1014, 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 1014 observations in 5 runs Run # start # end # total # 1 0 16 17 2 0 16 34 3 0 16 51 4 0 17 69 5 0 3 73 Total number of frames 73 130 unique data precomputed (should be 130) 130 unique data with 1014 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.8 (Out of 1014 removed 0 = 1014, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 1014 observations RMS deviation of equivalent data = 0.38998 Rint = 0.35172 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.34719, wR= 0.46124 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26107, wR= 0.34749, Acormin=0.523, Acormax=1.483, Acor_av=1.021 F test: Probability=1.000, F= 1.759 Trying model 2 (ne=2, no=1)... Results: Rint= 0.24975, wR= 0.34147, Acormin=0.556, Acormax=1.450, Acor_av=0.991 F test: Probability=0.896, F= 1.089 Trying model 3 (ne=4, no=0)... Results: Rint= 0.25617, wR= 0.34184, Acormin=0.531, Acormax=1.555, Acor_av=0.987 F test: Probability=0.658, F= 1.028 Trying model 4 (ne=4, no=1)... Results: Rint= 0.24078, wR= 0.33355, Acormin=0.485, Acormax=1.523, Acor_av=0.969 F test: Probability=0.985, F= 1.160 Trying model 5 (ne=4, no=3)... Results: Rint= 0.23285, wR= 0.31671, Acormin=0.304, Acormax=1.722, Acor_av=0.890 F test: Probability=0.806, F= 1.061 Trying model 6 (ne=6, no=0)... Results: Rint= 0.25188, wR= 0.32842, Acormin=0.263, Acormax=1.579, Acor_av=0.940 F test: Probability=0.000, F= 0.903 Trying model 7 (ne=6, no=1)... Results: Rint= 0.23728, wR= 0.31584, Acormin=0.276, Acormax=1.658, Acor_av=0.947 F test: Probability=0.582, F= 1.014 Trying model 8 (ne=6, no=3)... Results: Rint= 0.23533, wR= 0.30863, Acormin=0.220, Acormax=1.728, Acor_av=0.852 F test: Probability=0.628, F= 1.023 Trying model 9 (ne=6, no=5)... Results: Rint= 0.23287, wR= 0.30905, Acormin=0.278, Acormax=2.016, Acor_av=0.810 F test: Probability=0.670, F= 1.031 Trying model 10 (ne=8, no=0)... Results: Rint= 0.26589, wR= 0.32609, Acormin=0.053, Acormax=1.594, Acor_av=0.857 F test: Probability=0.000, F= 0.794 Trying model 11 (ne=8, no=1)... Results: Rint= 0.31149, wR= 0.36844, Acormin=0.050, Acormax=1.286, Acor_av=0.646 F test: Probability=0.000, F= 0.577 Trying model 12 (ne=8, no=3)... Results: Rint= 0.31728, wR= 0.37117, Acormin=-0.003, Acormax=0.110, Acor_av=0.042 F test: Probability=0.000, F= 0.551 Trying model 13 (ne=8, no=5)... Results: Rint= 0.29271, wR= 0.34961, Acormin=-0.002, Acormax=0.114, Acor_av=0.044 F test: Probability=0.000, F= 0.639 Trying model 14 (ne=8, no=7)... Results: Rint= 0.23299, wR= 0.30315, Acormin=0.003, Acormax=0.166, Acor_av=0.046 F test: Probability=0.000, F= 0.990 Final absorption model (ne=4, no=1): Rint= 0.24078, Acormin=0.485, Acormax=1.523, Acor_av=0.969 Combined refinement in use Rint: 0.36597 There are 73 active scales (one needs to be fixed) Refinement control: frame scale #39 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 1 (17 parameters) Refinement control: 89 pars with 4005 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.38998 Using Levenberg-Marquardt: 0.00010 New wR= 0.22715 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35172 with corrections 0.20329 Rint for all data: 0.36597 with corrections 0.21889 0 observations identified as outliers and rejected Cycle 2 wR= 0.22715 Using Levenberg-Marquardt: 0.00001 New wR= 0.21557 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35172 with corrections 0.19229 Rint for all data: 0.36597 with corrections 0.20803 0 observations identified as outliers and rejected Cycle 3 wR= 0.21557 Using Levenberg-Marquardt: 0.00000 New wR= 0.21264 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35172 with corrections 0.19127 Rint for all data: 0.36597 with corrections 0.20695 0 observations identified as outliers and rejected Cycle 4 wR= 0.21264 Using Levenberg-Marquardt: 0.00000 New wR= 0.21424 Using Levenberg-Marquardt: 0.00000 New wR= 0.21424 Using Levenberg-Marquardt: 0.00001 New wR= 0.21423 Using Levenberg-Marquardt: 0.00010 New wR= 0.21417 Using Levenberg-Marquardt: 0.00100 New wR= 0.21360 Using Levenberg-Marquardt: 0.01000 New wR= 0.21185 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35172 with corrections 0.18938 Rint for all data: 0.36597 with corrections 0.20508 0 observations identified as outliers and rejected Cycle 5 wR= 0.21185 Using Levenberg-Marquardt: 0.00100 New wR= 0.21581 Using Levenberg-Marquardt: 0.01000 New wR= 0.21264 Using Levenberg-Marquardt: 0.10000 New wR= 0.21128 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35172 with corrections 0.18871 Rint for all data: 0.36597 with corrections 0.20442 0 observations identified as outliers and rejected Final wR= 0.21128 Final frame scales: Min= 1.0000 Max= 4.3510 Final absorption correction factors: Amin= 0.3756 Amax= 1.7228 6 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=-1816.6368 max=1609600.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=30.5838 max=34715.7500 PROFFIT INFO: 2 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/104 4366 reflections read from tmp file 1082 reflections are rejected (1031 as outliers, 51 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 83 46 30 32 43 19 18 23 138 Initial Chi^2= 2.16522 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88415 Current error model SIG(F2)^2 = 470.04*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 415.59*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 415.59*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1609601- 115111 436 354714.53 31.56 100.00 114637- 3649 436 25773.89 6.74 81.42 3647- 1892 436 2518.69 2.61 27.29 1890- 1117 436 1473.65 2.00 18.58 1117- 724 436 913.31 1.34 1.38 724- 483 436 595.86 1.14 0.69 483- 293 436 382.09 1.02 0.69 292- 139 436 215.94 0.85 0.69 138- 17 436 73.62 0.50 0.23 16- -1817 442 -146.19 -0.32 0.00 ------------------------------------------------------------------------------------ 1609601- -1817 4366 38598.22 4.74 23.06 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 436 86456.11 10.53 53.67 1.75- 1.28 436 92525.71 9.54 39.91 1.28- 1.06 436 38920.89 5.12 28.67 1.06- 0.92 436 38875.92 4.12 17.43 0.92- 0.83 436 32961.15 4.09 17.66 0.83- 0.75 436 31337.20 3.77 18.35 0.75- 0.69 436 25061.36 3.41 16.51 0.69- 0.63 436 17300.41 2.63 13.53 0.63- 0.57 436 12103.80 2.12 12.61 0.57- 0.44 442 10821.88 2.06 12.44 ------------------------------------------------------------------------------------ 6.55- 0.44 4366 38598.22 4.74 23.06 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 436 86456.11 10.53 53.67 6.55- 1.28 872 89490.91 10.04 46.79 6.55- 1.06 1308 72634.24 8.40 40.75 6.55- 0.92 1744 64194.66 7.33 34.92 6.55- 0.83 2180 57947.96 6.68 31.47 6.55- 0.75 2616 53512.83 6.20 29.28 6.55- 0.69 3052 49448.34 5.80 27.46 6.55- 0.63 3488 45429.84 5.40 25.72 6.55- 0.57 3924 41726.95 5.04 24.26 6.55- 0.44 4366 38598.22 4.74 23.06 ------------------------------------------------------------------------------------ 6.55- 0.44 4366 38598.22 4.74 23.06 Scale applied to data: s=0.621271 (maximum obs:1609600.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.204; Rsigma 0.051: data 4366 -> merged 486 With outlier rejection... Rint 0.191; Rsigma 0.051: data 4301 -> merged 486 Rejected total: 65, method kkm 45, method Blessing 20 Completeness direct cell (a, b, c) = (6.563, 6.563, 6.563), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445549, 6.563352 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.59 22 22 23.45 100.00 516 1.55 - 1.22 22 22 21.14 100.00 465 1.20 - 1.03 22 22 18.73 100.00 412 1.03 - 0.92 22 22 15.27 100.00 336 0.92 - 0.84 22 22 15.36 100.00 338 0.84 - 0.79 22 22 12.45 100.00 274 0.79 - 0.75 22 22 12.41 100.00 273 0.75 - 0.71 22 22 9.77 100.00 215 0.71 - 0.69 22 22 10.14 100.00 223 0.68 - 0.65 27 29 9.04 93.10 244 --------------------------------------------------------------- 7.36 - 0.65 225 227 14.65 99.12 3296 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:55:20 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.376732 7.361469 7.369782 120.2044 120.1195 89.5381 4301 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.67 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2140 2154 2166 2151 3230 2849 2866 4301 N (int>3sigma) = 0 232 260 348 236 420 660 672 978 Mean intensity = 0.0 0.7 0.7 1.1 0.7 0.8 22.8 24.1 23.3 Mean int/sigma = 0.0 1.4 1.5 1.9 1.4 1.6 4.6 4.8 4.7 Lattice type: P chosen Volume: 282.73 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.343 7.360 7.361 119.71 119.84 90.19 Niggli form: a.a = 53.918 b.b = 54.169 c.c = 54.191 b.c = -26.856 a.c = -26.898 a.b = -0.177 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.401 CUBIC F-lattice R(int) = 0.235 [ 4062] Vol = 1130.9 Cell: 10.463 10.413 10.379 89.87 90.12 90.18 Volume: 1130.93 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.373 TETRAGONAL I-lattice R(int) = 0.220 [ 3676] Vol = 565.5 Cell: 7.392 7.370 10.379 90.01 89.82 89.73 Volume: 565.47 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.330 TETRAGONAL I-lattice R(int) = 0.207 [ 3671] Vol = 565.5 Cell: 7.343 7.360 10.463 89.79 90.04 90.19 Volume: 565.47 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.367 TETRAGONAL I-lattice R(int) = 0.220 [ 3676] Vol = 565.5 Cell: 7.370 7.392 10.379 90.18 90.01 90.27 Volume: 565.47 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.318 ORTHORHOMBIC F-lattice R(int) = 0.183 [ 3624] Vol = 1130.9 Cell: 10.379 10.413 10.463 90.18 90.12 89.87 Volume: 1130.93 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.440 ORTHORHOMBIC I-lattice R(int) = 0.181 [ 3601] Vol = 565.5 Cell: 10.379 7.370 7.392 89.73 89.82 90.01 Volume: 565.47 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.296 ORTHORHOMBIC I-lattice R(int) = 0.205 [ 3607] Vol = 565.5 Cell: 7.343 7.360 10.463 90.21 89.96 90.19 Volume: 565.47 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.264 MONOCLINIC I-lattice R(int) = 0.130 [ 3098] Vol = 565.5 Cell: 7.370 10.379 7.392 90.18 90.27 90.01 Volume: 565.47 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.279 MONOCLINIC I-lattice R(int) = 0.173 [ 3087] Vol = 565.5 Cell: 7.361 10.413 7.377 89.78 90.46 90.03 Volume: 565.47 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.263 MONOCLINIC I-lattice R(int) = 0.130 [ 3098] Vol = 565.5 Cell: 7.370 10.379 7.392 90.18 90.27 90.01 Volume: 565.47 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.187 MONOCLINIC I-lattice R(int) = 0.170 [ 3070] Vol = 565.5 Cell: 7.360 7.343 10.463 90.04 90.21 89.81 Volume: 565.47 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.143 MONOCLINIC I-lattice R(int) = 0.180 [ 3097] Vol = 565.5 Cell: 7.343 10.463 7.360 89.79 90.19 90.04 Volume: 565.47 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.257 MONOCLINIC I-lattice R(int) = 0.180 [ 3097] Vol = 565.5 Cell: 7.343 10.463 7.360 90.21 90.19 89.96 Volume: 565.47 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.124 [ 2114] Vol = 282.7 Cell: 7.343 7.360 7.361 119.71 119.84 90.19 Volume: 282.73 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 2166 0 2856 2865 4301 N (int>3sigma) = 0 0 0 0 348 0 672 675 978 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 23.6 24.1 23.3 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.7 4.9 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.759 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 27 27 312 849 N I>3s 0 0 0 203 0.0 0.0 -0.0 1.4 0.4 0.4 0.1 2.4 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 0.235 3778 Fd-3m 1 1 227 C N N N N 37 2284 0.235 3843 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.463410 10.413488 10.379396 89.8669 90.1187 90.1759 ZERR 1.00 0.000951 0.010470 0.005782 0.0037 0.0050 0.0938 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 823753- 94284 477 463 48 9.6 329120.07 29.82 0.175 0.203 92921- 2319 545 523 48 10.9 11548.34 4.24 0.296 0.158 2317- 1344 788 777 48 16.2 1875.63 2.12 0.863 1.002 1343- 924 689 686 48 14.3 1093.94 1.39 0.776 0.876 910- 712 410 406 48 8.5 792.97 1.10 0.608 0.684 710- 536 417 412 48 8.6 602.64 0.94 0.684 0.784 535- 428 358 355 48 7.4 472.95 0.82 0.695 0.765 427- 286 245 243 48 5.1 362.99 0.71 0.669 0.800 286- 127 267 266 48 5.5 193.61 0.51 0.842 1.165 122- -409 170 170 54 3.1 30.82 0.13 0.972 3.108 ------------------------------------------------------------------------------------------- 823753- -409 4366 4301 486 8.8 37552.49 4.67 0.191 0.211 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-1.14 1086 1064 48 22.2 75391.46 8.74 0.209 0.257 0.028 1.14-0.89 786 776 48 16.2 40749.85 4.78 0.171 0.182 0.053 0.89-0.76 659 652 49 13.3 32549.22 3.94 0.183 0.225 0.073 0.76-0.69 544 539 51 10.6 22398.79 3.12 0.171 0.205 0.081 0.69-0.63 402 398 48 8.3 18091.43 2.73 0.185 0.188 0.097 0.63-0.59 314 308 50 6.2 10444.35 1.98 0.204 0.222 0.125 0.58-0.55 226 221 48 4.6 15014.54 2.52 0.149 0.143 0.111 0.55-0.52 159 157 53 3.0 5486.33 1.39 0.092 0.086 0.167 0.52-0.49 122 119 50 2.4 12190.51 2.28 0.085 0.085 0.116 0.48-0.45 68 67 41 1.6 4960.23 1.17 0.418 0.515 0.183 ------------------------------------------------------------------------------------------------------ inf-0.45 4366 4301 486 8.8 37552.49 4.67 0.191 0.211 0.051 inf-0.65 3342 3296 225 14.6 44894.85 5.39 0.194 0.227 0.046 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-1.14 1064 48 48 100.0 22.2 75391.46 36.03 0.209 0.007 1.14-0.89 776 48 48 100.0 16.2 40749.85 16.12 0.171 0.017 0.89-0.76 652 49 49 100.0 13.3 32549.22 13.28 0.183 0.025 0.76-0.69 539 51 51 100.0 10.6 22398.79 9.58 0.171 0.029 0.69-0.63 398 50 48 96.0 8.3 18091.43 7.65 0.185 0.045 0.63-0.59 308 56 50 89.3 6.2 10444.35 4.74 0.204 0.055 0.58-0.55 221 55 48 87.3 4.6 15014.54 5.58 0.149 0.054 0.55-0.52 157 71 53 74.6 3.0 5486.33 2.40 0.092 0.091 0.52-0.49 119 84 50 59.5 2.4 12190.51 3.68 0.085 0.075 0.48-0.45 67 134 41 30.6 1.6 4960.23 1.47 0.418 0.956 -------------------------------------------------------------------------------------------- inf-0.45 4301 649 486 74.9 8.8 37552.49 16.58 0.191 0.025 inf-0.65 3296 227 225 99.1 14.6 44894.85 20.04 0.194 0.016 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 No constraint UB - matrix: 0.013110 -0.008908 -0.066367 ( 0.000011 0.000011 0.000010 ) 0.065190 -0.013082 0.014685 ( 0.000011 0.000011 0.000010 ) -0.014589 -0.066271 0.006114 ( 0.000014 0.000013 0.000012 ) M - matrix: 0.004634 -0.000003 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004642 -0.000006 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000006 0.004658 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.013110 -0.008908 -0.066367 ( 0.000011 0.000011 0.000010 ) 0.065190 -0.013082 0.014685 ( 0.000011 0.000011 0.000010 ) -0.014589 -0.066271 0.006114 ( 0.000014 0.000013 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4191(18) 10.4102(18) 10.3932(16) 89.925(13) 89.976(13) 89.965(14) V = 1127.3(3) unit cell: 10.4075(4) 10.4075(4) 10.4075(4) 90.0 90.0 90.0 V = 1127.30(8) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.172) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) Run 5 Omega scan: (-6.000 - 19.000,25 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-565.0000 max=7905880.0000 PROFFIT INFO: signal sum lp corr: min=-667.9608 max=1115295.6875 PROFFIT INFO: background sum: min=-77.0000 max=7581.0000 PROFFIT INFO: background sum sig2: min=394.0000 max=5651.0000 PROFFIT INFO: num of signal pixels: min=41 max=501 PROFFIT INFO: Inet: min=-1068.7372 max=1784473.0000 PROFFIT INFO: sig(Inet): min=49.1396 max=24370.5059 PROFFIT INFO: Inet/sig(Inet): min=-1.72 max=198.55 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 768 3064 4570 5468 5856 6812 7376 7730 8298 8642 8736 Percent 8.8 35.1 52.3 62.6 67.0 78.0 84.4 88.5 95.0 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4368 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 4368 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1784473- 127526 436 391871.80 75.79 100.00 126474- 3839 436 29247.40 19.51 100.00 3832- 2038 436 2786.04 7.02 97.94 2033- 1193 436 1555.23 3.84 50.46 1191- 797 436 977.34 2.26 12.61 795- 529 436 658.53 1.66 7.11 529- 327 436 423.71 1.25 5.73 327- 154 436 240.10 0.69 0.92 154- 17 436 81.69 0.29 0.00 16- -1069 444 -126.40 -0.25 0.00 ------------------------------------------------------------------------------------ 1784473- -1069 4368 42692.98 11.18 37.41 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 436 108263.26 14.96 67.66 1.73- 1.26 436 79469.27 21.12 60.55 1.26- 1.09 436 54949.48 17.80 64.22 1.09- 0.96 436 53182.35 14.94 36.93 0.96- 0.88 436 10687.31 5.44 39.45 0.88- 0.81 436 55030.61 15.60 38.07 0.81- 0.76 436 18216.30 5.68 17.20 0.76- 0.71 436 20832.87 6.86 17.89 0.71- 0.67 436 23535.05 7.86 27.29 0.67- 0.63 444 3482.72 1.75 5.41 ------------------------------------------------------------------------------------ 6.00- 0.63 4368 42692.98 11.18 37.41 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 13:55:21 2019 Sorting 4368 observations 43 unique observations with > 7.00 F2/sig(F2) 4368 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 103 411 5 0 24 436 Total number of frames 436 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 11 frame = 1 scale 4368 observations in 5 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 2 43 Total number of frames 43 1042 observations > 7.00 F2/sig(F2) 1042 observations in 5 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 2 43 Total number of frames 43 Removing 'redundancy=1' reflections Average redundancy: 20.0 (Out of 1042 removed 3 = 1039, unique = 52) 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 1039 observations in 5 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 2 43 Total number of frames 43 52 unique data precomputed (should be 52) 52 unique data with 1039 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.0 (Out of 1039 removed 0 = 1039, unique = 52) 52 unique data precomputed (should be 52) 52 unique data with 1039 observations RMS deviation of equivalent data = 0.27336 Rint = 0.19436 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18880, wR= 0.26038 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09685, wR= 0.14816, Acormin=0.592, Acormax=1.389, Acor_av=1.030 F test: Probability=1.000, F= 3.781 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09118, wR= 0.14031, Acormin=0.531, Acormax=1.445, Acor_av=1.003 F test: Probability=0.967, F= 1.125 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08177, wR= 0.13762, Acormin=0.598, Acormax=1.462, Acor_av=1.024 F test: Probability=1.000, F= 1.236 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08020, wR= 0.12650, Acormin=0.535, Acormax=1.575, Acor_av=1.001 F test: Probability=0.711, F= 1.036 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07320, wR= 0.11749, Acormin=0.574, Acormax=1.690, Acor_av=1.004 F test: Probability=0.999, F= 1.235 Final absorption model (ne=4, no=3): Rint= 0.07320, Acormin=0.574, Acormax=1.690, Acor_av=1.004 Combined refinement in use Rint: 0.19652 There are 43 active scales (one needs to be fixed) Refinement control: frame scale #11 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 66 pars with 2211 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.27336 Using Levenberg-Marquardt: 0.00010 New wR= 0.12366 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19436 with corrections 0.08763 Rint for all data: 0.19652 with corrections 0.09037 4 observations identified as outliers and rejected Cycle 2 wR= 0.10049 Using Levenberg-Marquardt: 0.00001 New wR= 0.08558 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18950 with corrections 0.05791 Rint for all data: 0.19652 with corrections 0.06656 1 observations identified as outliers and rejected Cycle 3 wR= 0.07885 Using Levenberg-Marquardt: 0.00000 New wR= 0.07750 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18899 with corrections 0.05565 Rint for all data: 0.19652 with corrections 0.06530 0 observations identified as outliers and rejected Cycle 4 wR= 0.07750 Using Levenberg-Marquardt: 0.00000 New wR= 0.07721 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18899 with corrections 0.05517 Rint for all data: 0.19652 with corrections 0.06492 0 observations identified as outliers and rejected Cycle 5 wR= 0.07721 Using Levenberg-Marquardt: 0.00000 New wR= 0.07710 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18899 with corrections 0.05497 Rint for all data: 0.19652 with corrections 0.06476 0 observations identified as outliers and rejected Final wR= 0.07710 Final frame scales: Min= 0.8157 Max= 1.1397 Final absorption correction factors: Amin= 0.4046 Amax= 1.5073 PROFFIT INFO: Inet (after scale3 abspack): min=-968.1025 max=1379632.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=48.3134 max=24395.8750 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/104 4368 reflections read from tmp file 194 reflections are rejected (193 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 2 6 0 7 3 4 4 133 Initial Chi^2= 0.51625 Cycle 1, Chi^2= 1.01676 Current error model SIG(F2)^2 = 67.30*I_RAW + 9.37*I_BACK+(0.03439*)^2 Cycle 2, Chi^2= 1.02548 Current error model SIG(F2)^2 = 83.75*I_RAW + 6.14*I_BACK+(0.02576*)^2 Cycle 3, Chi^2= 1.00589 Current error model SIG(F2)^2 = 88.31*I_RAW + 5.63*I_BACK+(0.02533*)^2 Cycle 4, Chi^2= 1.00090 Current error model SIG(F2)^2 = 89.13*I_RAW + 5.57*I_BACK+(0.02537*)^2 Cycle 5, Chi^2= 1.00018 Current error model SIG(F2)^2 = 89.28*I_RAW + 5.55*I_BACK+(0.02536*)^2 Final Chi^2= 1.00018 Final error model SIG(F2)^2 = 89.28*I_RAW + 5.55*I_BACK+(0.02536*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1379632- 116453 436 378793.25 31.36 100.00 116292- 3414 436 29230.18 12.87 100.00 3411- 2027 436 2665.12 5.90 99.54 2014- 1154 436 1519.33 3.92 64.22 1154- 768 436 930.13 2.63 18.81 768- 516 436 635.27 2.27 11.93 515- 322 436 413.33 1.94 9.86 322- 151 436 235.06 1.38 2.06 151- 17 436 81.90 0.73 0.23 17- -968 444 -123.90 -0.53 0.00 ------------------------------------------------------------------------------------ 1379632- -968 4368 41361.85 6.23 40.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 436 106794.47 10.15 70.87 1.73- 1.26 436 78005.87 9.47 63.07 1.26- 1.09 436 54713.79 8.02 68.58 1.09- 0.96 436 50158.46 6.89 39.45 0.96- 0.88 436 10505.10 4.08 45.18 0.88- 0.81 436 52671.17 8.27 42.66 0.81- 0.76 436 17068.86 3.75 19.04 0.76- 0.71 436 18983.35 4.79 19.95 0.71- 0.67 436 22048.37 5.32 31.65 0.67- 0.63 444 3366.20 1.69 6.08 ------------------------------------------------------------------------------------ 6.00- 0.63 4368 41361.85 6.23 40.59 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 436 106794.47 10.15 70.87 6.00- 1.26 872 92400.17 9.81 66.97 6.00- 1.09 1308 79838.04 9.21 67.51 6.00- 0.96 1744 72418.15 8.63 60.49 6.00- 0.88 2180 60035.54 7.72 57.43 6.00- 0.81 2616 58808.14 7.81 54.97 6.00- 0.76 3052 52845.39 7.23 49.84 6.00- 0.71 3488 48612.63 6.93 46.10 6.00- 0.67 3924 45661.05 6.75 44.50 6.00- 0.63 4368 41361.85 6.23 40.59 ------------------------------------------------------------------------------------ 6.00- 0.63 4368 41361.85 6.23 40.59 Scale applied to data: s=0.724830 (maximum obs:1379632.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.065; Rsigma 0.037: data 4368 -> merged 162 With outlier rejection... Rint 0.056; Rsigma 0.037: data 4351 -> merged 162 Rejected total: 17, method kkm 11, method Blessing 6 Completeness direct cell (a, b, c) = (10.407, 10.407, 10.407), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626457, 6.008769 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.36 - 1.76 14 14 28.64 100.00 401 1.73 - 1.27 14 14 31.71 100.00 444 1.26 - 1.06 14 14 35.50 100.00 497 1.05 - 0.97 14 14 30.57 100.00 428 0.95 - 0.88 14 14 32.14 100.00 450 0.87 - 0.81 14 14 28.64 100.00 401 0.80 - 0.76 14 14 29.86 100.00 418 0.76 - 0.72 14 14 25.07 100.00 351 0.72 - 0.69 14 14 27.21 100.00 381 0.69 - 0.65 19 19 23.16 100.00 440 --------------------------------------------------------------- 7.36 - 0.65 145 145 29.04 100.00 4211 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 13:55:20 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.376732 7.361469 7.369782 120.2044 120.1195 89.5381 4301 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.67 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2140 2154 2166 2151 3230 2849 2866 4301 N (int>3sigma) = 0 232 260 348 236 420 660 672 978 Mean intensity = 0.0 0.7 0.7 1.1 0.7 0.8 22.8 24.1 23.3 Mean int/sigma = 0.0 1.4 1.5 1.9 1.4 1.6 4.6 4.8 4.7 Lattice type: P chosen Volume: 282.73 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.343 7.360 7.361 119.71 119.84 90.19 Niggli form: a.a = 53.918 b.b = 54.169 c.c = 54.191 b.c = -26.856 a.c = -26.898 a.b = -0.177 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.401 CUBIC F-lattice R(int) = 0.235 [ 4062] Vol = 1130.9 Cell: 10.463 10.413 10.379 89.87 90.12 90.18 Volume: 1130.93 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.373 TETRAGONAL I-lattice R(int) = 0.220 [ 3676] Vol = 565.5 Cell: 7.392 7.370 10.379 90.01 89.82 89.73 Volume: 565.47 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.330 TETRAGONAL I-lattice R(int) = 0.207 [ 3671] Vol = 565.5 Cell: 7.343 7.360 10.463 89.79 90.04 90.19 Volume: 565.47 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.367 TETRAGONAL I-lattice R(int) = 0.220 [ 3676] Vol = 565.5 Cell: 7.370 7.392 10.379 90.18 90.01 90.27 Volume: 565.47 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.318 ORTHORHOMBIC F-lattice R(int) = 0.183 [ 3624] Vol = 1130.9 Cell: 10.379 10.413 10.463 90.18 90.12 89.87 Volume: 1130.93 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.440 ORTHORHOMBIC I-lattice R(int) = 0.181 [ 3601] Vol = 565.5 Cell: 10.379 7.370 7.392 89.73 89.82 90.01 Volume: 565.47 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.296 ORTHORHOMBIC I-lattice R(int) = 0.205 [ 3607] Vol = 565.5 Cell: 7.343 7.360 10.463 90.21 89.96 90.19 Volume: 565.47 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.264 MONOCLINIC I-lattice R(int) = 0.130 [ 3098] Vol = 565.5 Cell: 7.370 10.379 7.392 90.18 90.27 90.01 Volume: 565.47 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.279 MONOCLINIC I-lattice R(int) = 0.173 [ 3087] Vol = 565.5 Cell: 7.361 10.413 7.377 89.78 90.46 90.03 Volume: 565.47 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.263 MONOCLINIC I-lattice R(int) = 0.130 [ 3098] Vol = 565.5 Cell: 7.370 10.379 7.392 90.18 90.27 90.01 Volume: 565.47 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.187 MONOCLINIC I-lattice R(int) = 0.170 [ 3070] Vol = 565.5 Cell: 7.360 7.343 10.463 90.04 90.21 89.81 Volume: 565.47 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.143 MONOCLINIC I-lattice R(int) = 0.180 [ 3097] Vol = 565.5 Cell: 7.343 10.463 7.360 89.79 90.19 90.04 Volume: 565.47 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.257 MONOCLINIC I-lattice R(int) = 0.180 [ 3097] Vol = 565.5 Cell: 7.343 10.463 7.360 90.21 90.19 89.96 Volume: 565.47 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.124 [ 2114] Vol = 282.7 Cell: 7.343 7.360 7.361 119.71 119.84 90.19 Volume: 282.73 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 2166 0 2856 2865 4301 N (int>3sigma) = 0 0 0 0 348 0 672 675 978 Mean intensity = 0.0 0.0 0.0 0.0 1.1 0.0 23.6 24.1 23.3 Mean int/sigma = 0.0 0.0 0.0 0.0 1.9 0.0 4.7 4.9 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.759 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 27 27 312 849 N I>3s 0 0 0 203 0.0 0.0 -0.0 1.4 0.4 0.4 0.1 2.4 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 0.235 3778 Fd-3m 1 1 227 C N N N N 37 2284 0.235 3843 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.463410 10.413488 10.379396 89.8669 90.1187 90.1759 ZERR 1.00 0.000951 0.010470 0.005782 0.0037 0.0050 0.0938 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1157025- 91802 533 523 27 19.4 330758.18 29.44 0.052 0.065 75888- 1704 886 882 27 32.7 4979.30 7.85 0.105 0.141 1531- 769 801 799 27 29.6 1073.68 2.74 0.243 0.311 707- 320 903 903 27 33.4 483.23 1.89 0.382 0.532 319- 77 588 587 27 21.7 216.74 1.16 0.619 1.025 73- -202 657 657 27 24.3 12.35 0.19 0.956 3.818 ------------------------------------------------------------------------------------------- 1157025- -202 4368 4351 162 26.9 41095.80 6.21 0.056 0.070 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-1.27 847 843 27 31.2 94341.55 10.03 0.050 0.061 0.028 1.26-0.97 928 925 28 33.0 49069.88 7.05 0.048 0.065 0.034 0.95-0.81 854 851 28 30.4 32122.42 6.26 0.059 0.074 0.043 0.80-0.73 751 750 27 27.8 17492.10 4.17 0.076 0.095 0.055 0.72-0.67 665 664 27 24.6 18291.91 4.54 0.086 0.110 0.063 0.66-0.63 323 318 25 12.7 4047.76 1.82 0.144 0.099 0.124 ------------------------------------------------------------------------------------------------------ inf-0.63 4368 4351 162 26.9 41095.80 6.21 0.056 0.070 0.037 inf-0.65 4223 4209 144 29.2 42245.93 6.35 0.055 0.068 0.037 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-1.27 843 27 27 100.0 31.2 94341.55 53.77 0.050 0.007 1.26-0.97 925 28 28 100.0 33.0 49069.88 38.31 0.048 0.007 0.95-0.81 851 28 28 100.0 30.4 32122.42 34.98 0.059 0.010 0.80-0.73 750 27 27 100.0 27.8 17492.10 20.08 0.076 0.012 0.72-0.67 664 27 27 100.0 24.6 18291.91 24.37 0.086 0.013 0.66-0.63 318 25 25 100.0 12.7 4047.76 6.86 0.144 0.038 -------------------------------------------------------------------------------------------- inf-0.63 4351 162 162 100.0 26.9 41095.80 33.09 0.056 0.009 inf-0.65 4209 144 144 100.0 29.2 42245.93 34.00 0.055 0.009 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:01:59 2019) ID: 3668; threads 40; handles 811; mem 515332.00 (1204688.00)kB; time: 1w 5d 0h 12m 47s MEMORY INFO: Memory PF:223.0, Ph:556.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.3,peak PF: 700.2, WS: 471.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:224.0, Ph:558.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.0,peak PF: 700.2, WS: 473.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:01:59 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000083 0.000065 0.000084 ) 0.064809 0.092374 0.027273 ( 0.000097 0.000076 0.000098 ) 0.045523 0.057900 0.132205 ( 0.000117 0.000092 0.000119 ) 7.38096 ( 0.00648 ) 7.36649 ( 0.00699 ) 7.42630 ( 0.00798 ) 120.52449 ( 0.10786 ) 120.40327 ( 0.10371 ) 89.27095 ( 0.07399 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 14:01:59 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000083 0.000065 0.000084 ) 0.064809 0.092374 0.027273 ( 0.000097 0.000076 0.000098 ) 0.045523 0.057900 0.132205 ( 0.000117 0.000092 0.000119 ) M - matrix: 0.013770 0.004509 0.009166 ( 0.000022 0.000015 0.000019 ) 0.004509 0.013966 0.009337 ( 0.000015 0.000019 0.000017 ) 0.009166 0.009337 0.018550 ( 0.000019 0.000017 0.000032 ) unit cell: 7.381(6) 7.366(7) 7.426(8) 120.52(11) 120.40(10) 89.27(7) V = 283.3(5) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.82 | 24 | 1.005 ( 0.047) | 1.008 ( 0.130) | 0.907 ( 0.354) | 0.79- 0.69 | 24 | 0.998 ( 0.044) | 1.006 ( 0.137) | 1.289 ( 0.497) | 0.69- 0.63 | 23 | 0.979 ( 0.051) | 0.913 ( 0.103) | 1.157 ( 0.432) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.510) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 46 obs out of 238 (total:238,skipped:0) (19.33%) UB - matrix: 0.086322 -0.045974 0.017116 ( 0.000473 0.000165 0.000229 ) 0.064318 0.092941 0.027760 ( 0.000633 0.000220 0.000306 ) 0.045617 0.058321 0.132889 ( 0.000830 0.000289 0.000401 ) M - matrix: 0.013669 0.004670 0.009325 ( 0.000138 0.000083 0.000117 ) 0.004670 0.014153 0.009543 ( 0.000083 0.000055 0.000055 ) 0.009325 0.009543 0.018723 ( 0.000117 0.000055 0.000108 ) unit cell: 7.47(3) 7.36(3) 7.42(3) 120.7(5) 120.4(5) 89.5(4) V = 285(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 4, #refl in peak table: 238 #indexed refl 216, indexation with best UB: 90.7563% Lattice: 7.4072 7.3556 7.3610 120.005 120.354 89.764 282.632 Rotation: -22.660 24.759 -35.022 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 227 obs out of 238 (total:238,skipped:0) (95.38%) UB - matrix: 0.087760 -0.044390 0.012681 ( 0.000052 0.000055 0.000059 ) 0.061495 0.094382 0.026268 ( 0.000060 0.000065 0.000069 ) 0.049386 0.055440 0.133261 ( 0.000059 0.000063 0.000067 ) M - matrix: 0.013922 0.004646 0.009310 ( 0.000013 0.000010 0.000011 ) 0.004646 0.013952 0.009304 ( 0.000010 0.000015 0.000012 ) 0.009310 0.009304 0.018609 ( 0.000011 0.000012 0.000018 ) unit cell: 7.369(4) 7.355(5) 7.360(5) 120.01(7) 120.09(6) 89.95(5) V = 281.8(3) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1316 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 223 peaks identified as outliers and rejected 223 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 223 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 223 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 2.38 | 22 | 0.899 ( 0.094) | 0.905 ( 0.131) | 0.958 ( 0.493) | 2.38- 1.83 | 22 | 0.900 ( 0.110) | 0.921 ( 0.154) | 0.939 ( 0.269) | 1.76- 1.58 | 22 | 0.887 ( 0.115) | 0.904 ( 0.161) | 0.806 ( 0.264) | 1.58- 1.35 | 22 | 0.954 ( 0.082) | 0.983 ( 0.130) | 0.791 ( 0.395) | 1.35- 1.19 | 22 | 0.935 ( 0.082) | 0.954 ( 0.100) | 0.903 ( 0.428) | 1.19- 1.00 | 22 | 0.962 ( 0.087) | 0.981 ( 0.123) | 0.884 ( 0.304) | 1.00- 0.88 | 22 | 0.988 ( 0.064) | 0.995 ( 0.081) | 1.052 ( 0.398) | 0.88- 0.79 | 22 | 0.993 ( 0.048) | 0.994 ( 0.129) | 0.938 ( 0.310) | 0.79- 0.69 | 22 | 0.975 ( 0.044) | 0.932 ( 0.088) | 1.196 ( 0.465) | 0.69- 0.63 | 25 | 0.933 ( 0.047) | 0.852 ( 0.068) | 1.275 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 0.63 | 223 | 0.942 ( 0.089) | 0.941 ( 0.128) | 0.978 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) UB - matrix: 0.088106 -0.044293 0.012828 ( 0.000028 0.000032 0.000033 ) 0.061394 0.094519 0.026063 ( 0.000022 0.000026 0.000027 ) 0.049283 0.055378 0.133130 ( 0.000021 0.000024 0.000025 ) M - matrix: 0.013961 0.004630 0.009291 ( 0.000006 0.000004 0.000005 ) 0.004630 0.013962 0.009268 ( 0.000004 0.000006 0.000005 ) 0.009291 0.009268 0.018567 ( 0.000005 0.000005 0.000007 ) unit cell: 7.351(2) 7.341(2) 7.3536(18) 119.91(3) 120.04(3) 89.95(2) V = 280.88(13) OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 UB - matrix: 0.087896 -0.044356 0.012683 ( 0.000021 0.000024 0.000025 ) 0.061495 0.094417 0.026185 ( 0.000020 0.000022 0.000024 ) 0.049387 0.055447 0.133218 ( 0.000019 0.000022 0.000023 ) M - matrix: 0.013946 0.004646 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013956 0.009296 ( 0.000004 0.000005 0.000004 ) 0.009304 0.009296 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3589(17) 7.3517(18) 7.3584(16) 119.99(2) 120.05(2) 89.96(2) V = 281.42(11) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087896 -0.044356 0.012683 ( 0.000021 0.000024 0.000025 ) 0.061495 0.094417 0.026185 ( 0.000020 0.000022 0.000024 ) 0.049387 0.055447 0.133218 ( 0.000019 0.000022 0.000023 ) M - matrix: 0.013946 0.004646 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013956 0.009296 ( 0.000004 0.000005 0.000004 ) 0.009304 0.009296 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3589(17) 7.3517(18) 7.3584(16) 119.99(2) 120.05(2) 89.96(2) V = 281.42(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) 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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 223 peaks identified as outliers and rejected 223 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 223 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 223 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 22 | 0.868 ( 0.103) | 0.880 ( 0.128) | 0.911 ( 0.399) | 2.38- 1.83 | 22 | 0.907 ( 0.104) | 0.924 ( 0.157) | 0.918 ( 0.259) | 1.76- 1.59 | 22 | 0.880 ( 0.117) | 0.891 ( 0.164) | 0.729 ( 0.225) | 1.58- 1.45 | 22 | 0.947 ( 0.083) | 0.969 ( 0.129) | 0.883 ( 0.461) | 1.45- 1.19 | 22 | 0.926 ( 0.075) | 0.944 ( 0.084) | 0.839 ( 0.422) | 1.19- 1.06 | 22 | 0.980 ( 0.083) | 1.000 ( 0.124) | 0.894 ( 0.363) | 1.01- 0.88 | 22 | 0.983 ( 0.064) | 1.014 ( 0.078) | 1.039 ( 0.371) | 0.88- 0.79 | 22 | 0.991 ( 0.048) | 0.987 ( 0.128) | 0.966 ( 0.330) | 0.79- 0.69 | 22 | 0.976 ( 0.044) | 0.935 ( 0.090) | 1.283 ( 0.490) | 0.69- 0.63 | 25 | 0.933 ( 0.048) | 0.854 ( 0.073) | 1.273 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 223 | 0.939 ( 0.090) | 0.939 ( 0.130) | 0.977 ( 0.421) | 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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb PROFFITPEAK info: 208 peaks in the peak location table UB fit with 38 obs out of 126 (total:126,skipped:0) (30.16%) UB - matrix: 0.087591 -0.046288 0.017322 ( 0.000241 0.000776 0.000276 ) 0.064457 0.092166 0.027187 ( 0.000255 0.000823 0.000293 ) 0.045908 0.059255 0.132588 ( 0.000361 0.001166 0.000415 ) M - matrix: 0.013934 0.004607 0.009357 ( 0.000063 0.000107 0.000061 ) 0.004607 0.014148 0.009561 ( 0.000107 0.000217 0.000161 ) 0.009357 0.009561 0.018619 ( 0.000061 0.000161 0.000111 ) unit cell: 7.38(4) 7.38(5) 7.47(5) 121.2(7) 120.5(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 5, #refl in peak table: 126 #indexed refl 114, indexation with best UB: 90.4762% Lattice: 7.3629 7.3310 7.3524 120.038 120.202 89.606 280.561 Rotation: -22.722 24.645 -34.978 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 118 obs out of 126 (total:126,skipped:0) (93.65%) UB - matrix: 0.087826 -0.044605 0.012486 ( 0.000053 0.000105 0.000055 ) 0.061468 0.094488 0.026051 ( 0.000058 0.000115 0.000060 ) 0.049297 0.055225 0.133174 ( 0.000037 0.000074 0.000039 ) M - matrix: 0.013922 0.004613 0.009263 ( 0.000012 0.000014 0.000008 ) 0.004613 0.013967 0.009259 ( 0.000014 0.000025 0.000012 ) 0.009263 0.009259 0.018570 ( 0.000008 0.000012 0.000011 ) unit cell: 7.355(6) 7.335(7) 7.345(4) 119.89(8) 119.99(7) 89.97(7) V = 280.8(4) OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 UB fit with 118 obs out of 126 (total:126,skipped:0) (93.65%) UB - matrix: 0.087832 -0.044599 0.012475 ( 0.000051 0.000102 0.000054 ) 0.061473 0.094490 0.026044 ( 0.000059 0.000117 0.000061 ) 0.049302 0.055220 0.133166 ( 0.000038 0.000075 0.000039 ) M - matrix: 0.013924 0.004614 0.009262 ( 0.000012 0.000014 0.000008 ) 0.004614 0.013967 0.009258 ( 0.000014 0.000025 0.000012 ) 0.009262 0.009258 0.018567 ( 0.000008 0.000012 0.000011 ) unit cell: 7.354(6) 7.335(7) 7.345(4) 119.88(8) 119.98(7) 89.97(7) V = 280.8(4) OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 OTKP changes: 48 1 1 1 UB - matrix: 0.087849 -0.044593 0.012493 ( 0.000051 0.000102 0.000053 ) 0.061480 0.094509 0.026053 ( 0.000059 0.000117 0.000061 ) 0.049325 0.055238 0.133193 ( 0.000038 0.000076 0.000040 ) M - matrix: 0.013930 0.004618 0.009269 ( 0.000012 0.000014 0.000008 ) 0.004618 0.013972 0.009262 ( 0.000014 0.000025 0.000013 ) 0.009269 0.009262 0.018575 ( 0.000008 0.000013 0.000011 ) UB fit with 118 obs out of 126 (total:126,skipped:0) (93.65%) unit cell: 7.353(6) 7.334(7) 7.344(4) 119.88(8) 119.99(7) 89.97(7) V = 280.7(4) 126 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Run 5 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087849 -0.044593 0.012493 ( 0.000051 0.000102 0.000053 ) 0.061480 0.094509 0.026053 ( 0.000059 0.000117 0.000061 ) 0.049325 0.055238 0.133193 ( 0.000038 0.000076 0.000040 ) M - matrix: 0.013930 0.004618 0.009269 ( 0.000012 0.000014 0.000008 ) 0.004618 0.013972 0.009262 ( 0.000014 0.000025 0.000013 ) 0.009269 0.009262 0.018575 ( 0.000008 0.000013 0.000011 ) UB fit with 118 obs out of 126 (total:126,skipped:0) (93.65%) unit cell: 7.353(6) 7.334(7) 7.344(4) 119.88(8) 119.99(7) 89.97(7) V = 280.7(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 118 obs out of 126 (total:126,skipped:0) (93.65%) 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= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb 0 of 114 peaks identified as outliers and rejected 114 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 114 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 114 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.13 | 11 | 0.869 ( 0.110) | 0.860 ( 0.135) | 0.879 ( 0.209) | 2.12- 1.75 | 11 | 0.900 ( 0.125) | 1.058 ( 0.399) | 0.997 ( 0.576) | 1.75- 1.57 | 11 | 0.963 ( 0.116) | 0.960 ( 0.139) | 0.935 ( 0.363) | 1.57- 1.35 | 11 | 0.980 ( 0.094) | 0.979 ( 0.141) | 0.813 ( 0.373) | 1.35- 1.20 | 11 | 0.973 ( 0.074) | 0.997 ( 0.138) | 0.886 ( 0.281) | 1.20- 1.09 | 11 | 1.000 ( 0.059) | 0.998 ( 0.110) | 0.901 ( 0.303) | 1.09- 1.00 | 11 | 0.995 ( 0.086) | 1.021 ( 0.113) | 0.900 ( 0.476) | 0.97- 0.87 | 11 | 1.011 ( 0.079) | 0.988 ( 0.116) | 1.011 ( 0.261) | 0.86- 0.78 | 11 | 1.031 ( 0.051) | 1.066 ( 0.145) | 0.950 ( 0.250) | 0.75- 0.65 | 15 | 1.021 ( 0.041) | 0.973 ( 0.101) | 1.119 ( 0.409) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.65 | 114 | 0.976 ( 0.100) | 0.989 ( 0.181) | 0.946 ( 0.378) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 114 obs out of 114 (total:114,skipped:0) (100.00%) UB - matrix: 0.088053 -0.044544 0.012712 ( 0.000027 0.000053 0.000028 ) 0.061638 0.094670 0.026400 ( 0.000047 0.000093 0.000050 ) 0.049403 0.055303 0.133262 ( 0.000023 0.000045 0.000024 ) M - matrix: 0.013993 0.004645 0.009330 ( 0.000008 0.000009 0.000005 ) 0.004645 0.014005 0.009303 ( 0.000009 0.000019 0.000008 ) 0.009330 0.009303 0.018617 ( 0.000005 0.000008 0.000007 ) unit cell: 7.348(4) 7.333(5) 7.353(3) 119.95(6) 120.12(5) 89.90(5) V = 280.1(3) OTKP changes: 114 1 1 1 OTKP changes: 114 1 1 1 OTKP changes: 114 1 1 1 UB - matrix: 0.087851 -0.044606 0.012532 ( 0.000025 0.000049 0.000027 ) 0.061574 0.094530 0.026251 ( 0.000042 0.000082 0.000044 ) 0.049330 0.055265 0.133195 ( 0.000022 0.000043 0.000023 ) M - matrix: 0.013942 0.004628 0.009288 ( 0.000007 0.000008 0.000005 ) 0.004628 0.013980 0.009283 ( 0.000008 0.000017 0.000008 ) 0.009288 0.009283 0.018587 ( 0.000005 0.000008 0.000007 ) UB fit with 114 obs out of 114 (total:114,skipped:0) (100.00%) unit cell: 7.355(3) 7.338(5) 7.351(3) 119.94(5) 120.03(4) 89.93(4) V = 280.8(2) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 730 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087851 -0.044606 0.012532 ( 0.000025 0.000049 0.000027 ) 0.061574 0.094530 0.026251 ( 0.000042 0.000082 0.000044 ) 0.049330 0.055265 0.133195 ( 0.000022 0.000043 0.000023 ) M - matrix: 0.013942 0.004628 0.009288 ( 0.000007 0.000008 0.000005 ) 0.004628 0.013980 0.009283 ( 0.000008 0.000017 0.000008 ) 0.009288 0.009283 0.018587 ( 0.000005 0.000008 0.000007 ) UB fit with 114 obs out of 114 (total:114,skipped:0) (100.00%) unit cell: 7.355(3) 7.338(5) 7.351(3) 119.94(5) 120.03(4) 89.93(4) V = 280.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 114 obs out of 114 (total:114,skipped:0) (100.00%) 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= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb 0 of 115 peaks identified as outliers and rejected 115 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 115 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 115 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 2.37 | 12 | 0.873 ( 0.111) | 0.881 ( 0.156) | 0.804 ( 0.177) | 2.12- 1.75 | 12 | 0.891 ( 0.143) | 1.032 ( 0.363) | 0.963 ( 0.500) | 1.75- 1.56 | 12 | 0.962 ( 0.112) | 0.968 ( 0.135) | 0.983 ( 0.462) | 1.56- 1.35 | 12 | 1.016 ( 0.067) | 1.045 ( 0.092) | 0.891 ( 0.418) | 1.35- 1.19 | 12 | 0.959 ( 0.089) | 0.973 ( 0.163) | 0.751 ( 0.337) | 1.19- 1.00 | 12 | 0.994 ( 0.064) | 0.995 ( 0.094) | 0.989 ( 0.323) | 1.00- 0.88 | 12 | 1.006 ( 0.086) | 0.994 ( 0.113) | 0.971 ( 0.365) | 0.88- 0.82 | 12 | 1.025 ( 0.059) | 1.038 ( 0.113) | 1.076 ( 0.313) | 0.79- 0.69 | 12 | 1.041 ( 0.036) | 0.994 ( 0.120) | 1.069 ( 0.392) | 0.69- 0.65 | 7 | 1.007 ( 0.040) | 0.992 ( 0.129) | 1.095 ( 0.371) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 0.65 | 115 | 0.976 ( 0.104) | 0.991 ( 0.173) | 0.953 ( 0.391) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.0 | 104 | 0.988 ( 0.039) | 1.031 ( 0.066) | 1.119 ( 0.484) | 10.1-14.6 | 104 | 0.989 ( 0.046) | 1.043 ( 0.070) | 1.135 ( 0.520) | 14.7-18.8 | 104 | 0.997 ( 0.207) | 1.026 ( 0.095) | 1.176 ( 1.082) | 18.8-23.5 | 104 | 0.964 ( 0.058) | 1.003 ( 0.081) | 0.940 ( 0.408) | 23.5-27.0 | 104 | 0.965 ( 0.062) | 0.994 ( 0.091) | 0.947 ( 0.420) | 27.1-32.4 | 104 | 0.950 ( 0.086) | 0.966 ( 0.115) | 0.931 ( 0.447) | 32.4-36.3 | 104 | 0.926 ( 0.157) | 0.907 ( 0.131) | 1.057 ( 0.629) | 36.3-38.8 | 104 | 0.881 ( 0.095) | 0.849 ( 0.128) | 1.007 ( 0.477) | 38.8-41.8 | 104 | 0.896 ( 0.099) | 0.863 ( 0.181) | 1.057 ( 0.473) | 41.9-50.1 | 107 | 0.872 ( 0.118) | 0.796 ( 0.133) | 0.932 ( 0.471) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1043 | 0.943 ( 0.118) | 0.947 ( 0.142) | 1.030 ( 0.580) | Fitted profile normalization line parameters e1 dimension: a=-0.0035 b=1.14 e2 dimension: a=-0.0070 b=1.24 e3 dimension: a=0.0003 b=1.09 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3814 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1574740 PROFFITPEAK - Finished at Wed Aug 21 14:02:14 2019 PROFFITMAIN - Started at Wed Aug 21 14:02:14 2019 OTKP changes: 389 2 4 5 OTKP changes: 389 2 4 5 OTKP changes: 389 2 4 5 UB - matrix: 0.087785 -0.046041 0.016631 ( 0.000070 0.000062 0.000074 ) 0.062891 0.092284 0.026676 ( 0.000080 0.000070 0.000084 ) 0.045344 0.057601 0.132040 ( 0.000086 0.000076 0.000091 ) M - matrix: 0.013718 0.004374 0.009125 ( 0.000018 0.000012 0.000015 ) 0.004374 0.013954 0.009302 ( 0.000012 0.000017 0.000014 ) 0.009125 0.009302 0.018423 ( 0.000015 0.000014 0.000025 ) UB fit with 464 obs out of 1043 (total:1043,skipped:0) (44.49%) unit cell: 7.398(6) 7.374(6) 7.436(6) 120.88(9) 120.36(8) 88.55(6) V = 285.0(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 193 obs out of 212 (total:212,skipped:0) (91.04%) UB - matrix: 0.087749 -0.046156 0.017211 ( 0.000107 0.000066 0.000103 ) 0.064366 0.092331 0.027080 ( 0.000099 0.000061 0.000095 ) 0.045614 0.057703 0.131950 ( 0.000119 0.000073 0.000115 ) M - matrix: 0.013923 0.004525 0.009272 ( 0.000025 0.000015 0.000020 ) 0.004525 0.013985 0.009320 ( 0.000015 0.000015 0.000016 ) 0.009272 0.009320 0.018440 ( 0.000020 0.000016 0.000031 ) unit cell: 7.372(7) 7.366(7) 7.441(8) 120.60(10) 120.45(11) 89.00(8) V = 283.6(5) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 UB - matrix: 0.087303 -0.045977 0.017386 ( 0.000098 0.000061 0.000092 ) 0.064696 0.092341 0.027291 ( 0.000085 0.000053 0.000080 ) 0.045545 0.057817 0.131999 ( 0.000103 0.000064 0.000097 ) M - matrix: 0.013882 0.004593 0.009295 ( 0.000022 0.000013 0.000017 ) 0.004593 0.013984 0.009353 ( 0.000013 0.000013 0.000013 ) 0.009295 0.009353 0.018471 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.394(6) 7.376(6) 7.441(6) 120.53(9) 120.41(9) 89.30(7) V = 284.6(4) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.161) HKL list info: 1289 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087298 -0.045975 0.017390 ( 0.000098 0.000061 0.000092 ) 0.064687 0.092343 0.027293 ( 0.000087 0.000054 0.000082 ) 0.045493 0.057822 0.131992 ( 0.000103 0.000064 0.000097 ) M - matrix: 0.013875 0.004590 0.009288 ( 0.000022 0.000013 0.000017 ) 0.004590 0.013984 0.009353 ( 0.000013 0.000014 0.000013 ) 0.009288 0.009353 0.018469 ( 0.000017 0.000013 0.000026 ) UB fit with 199 obs out of 212 (total:212,skipped:0) (93.87%) unit cell: 7.394(6) 7.376(6) 7.441(6) 120.54(9) 120.39(9) 89.30(7) V = 284.6(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.117978 0.039139 0.078705 ( 0.000076 0.000047 0.000070 ) 0.000022 0.111519 0.056248 ( 0.000077 0.000048 0.000071 ) 0.000037 -0.000044 0.095469 ( 0.000089 0.000056 0.000083 ) M - matrix: 0.013919 0.004620 0.009290 ( 0.000018 0.000011 0.000014 ) 0.004620 0.013968 0.009349 ( 0.000011 0.000011 0.000011 ) 0.009290 0.009349 0.018473 ( 0.000014 0.000011 0.000021 ) UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) unit cell: 7.377(5) 7.380(5) 7.429(8) 120.48(9) 120.25(9) 89.49(6) V = 284.1(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.087804 -0.044309 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094149 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055798 0.133161 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004658 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009312 0.018585 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3551(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1268 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) UB - matrix: 0.087903 -0.044369 0.012678 ( 0.000021 0.000024 0.000026 ) 0.061483 0.094414 0.026172 ( 0.000019 0.000022 0.000023 ) 0.049390 0.055433 0.133214 ( 0.000017 0.000020 0.000021 ) M - matrix: 0.013947 0.004643 0.009303 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013955 0.009293 ( 0.000004 0.000005 0.000004 ) 0.009303 0.009293 0.018592 ( 0.000004 0.000004 0.000006 ) unit cell: 7.3585(17) 7.3510(18) 7.3581(15) 119.98(2) 120.05(2) 89.95(2) V = 281.39(11) OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1296 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087903 -0.044369 0.012678 ( 0.000021 0.000024 0.000026 ) 0.061483 0.094414 0.026172 ( 0.000019 0.000022 0.000023 ) 0.049390 0.055433 0.133214 ( 0.000017 0.000020 0.000021 ) M - matrix: 0.013947 0.004643 0.009303 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013955 0.009293 ( 0.000004 0.000005 0.000004 ) 0.009303 0.009293 0.018592 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3585(17) 7.3510(18) 7.3581(15) 119.98(2) 120.05(2) 89.95(2) V = 281.39(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* UB - matrix: 0.118100 0.039327 0.078777 ( 0.000021 0.000024 0.000026 ) 0.000003 0.111393 0.055619 ( 0.000011 0.000012 0.000013 ) -0.000002 0.000003 0.096401 ( 0.000023 0.000027 0.000029 ) M - matrix: 0.013948 0.004645 0.009304 ( 0.000005 0.000003 0.000004 ) 0.004645 0.013955 0.009294 ( 0.000003 0.000003 0.000004 ) 0.009304 0.009294 0.018592 ( 0.000004 0.000004 0.000007 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3582(16) 7.3514(13) 7.358(3) 119.98(3) 120.05(3) 89.965(17) V = 281.39(12) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) UB - matrix: 0.087859 -0.044597 0.012540 ( 0.000025 0.000048 0.000026 ) 0.061574 0.094539 0.026257 ( 0.000042 0.000082 0.000044 ) 0.049347 0.055267 0.133189 ( 0.000021 0.000041 0.000022 ) M - matrix: 0.013946 0.004630 0.009291 ( 0.000007 0.000008 0.000005 ) 0.004630 0.013981 0.009284 ( 0.000008 0.000017 0.000007 ) 0.009291 0.009284 0.018586 ( 0.000005 0.000007 0.000006 ) unit cell: 7.355(3) 7.338(5) 7.352(3) 119.94(5) 120.04(4) 89.93(4) V = 280.8(2) OTKP changes: 115 1 1 1 OTKP changes: 115 1 1 1 OTKP changes: 115 1 1 1 OTKP changes: 115 1 1 1 UB - matrix: 0.087857 -0.044598 0.012538 ( 0.000025 0.000048 0.000026 ) 0.061573 0.094537 0.026256 ( 0.000042 0.000082 0.000044 ) 0.049345 0.055266 0.133186 ( 0.000021 0.000041 0.000022 ) M - matrix: 0.013945 0.004630 0.009290 ( 0.000007 0.000008 0.000005 ) 0.004630 0.013981 0.009284 ( 0.000008 0.000017 0.000007 ) 0.009290 0.009284 0.018585 ( 0.000005 0.000007 0.000006 ) UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) unit cell: 7.355(3) 7.338(5) 7.352(3) 119.94(5) 120.04(4) 89.93(4) V = 280.8(2) Run 5 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 708 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087857 -0.044598 0.012538 ( 0.000025 0.000048 0.000026 ) 0.061573 0.094537 0.026256 ( 0.000042 0.000082 0.000044 ) 0.049345 0.055266 0.133186 ( 0.000021 0.000041 0.000022 ) M - matrix: 0.013945 0.004630 0.009290 ( 0.000007 0.000008 0.000005 ) 0.004630 0.013981 0.009284 ( 0.000008 0.000017 0.000007 ) 0.009290 0.009284 0.018585 ( 0.000005 0.000007 0.000006 ) UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) unit cell: 7.355(3) 7.338(5) 7.352(3) 119.94(5) 120.04(4) 89.93(4) V = 280.8(2) 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! *** Best per run unit cell (run 5) ******* UB - matrix: 0.087857 -0.044598 0.012538 ( 0.000025 0.000048 0.000026 ) 0.061573 0.094537 0.026256 ( 0.000042 0.000082 0.000044 ) 0.049345 0.055266 0.133186 ( 0.000021 0.000041 0.000022 ) M - matrix: 0.013945 0.004630 0.009290 ( 0.000007 0.000008 0.000005 ) 0.004630 0.013981 0.009284 ( 0.000008 0.000017 0.000007 ) 0.009290 0.009284 0.018585 ( 0.000005 0.000007 0.000006 ) UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) unit cell: 7.355(3) 7.338(5) 7.352(3) 119.94(5) 120.04(4) 89.93(4) V = 280.8(2) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 69.89 ph= 92.09 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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117598 0.038399 0.078531 ( 0.000042 0.000043 0.000049 ) -0.000001 0.111510 0.056194 ( 0.000027 0.000027 0.000031 ) -0.000037 -0.000104 0.096187 ( 0.000025 0.000025 0.000029 ) M - matrix: 0.013829 0.004516 0.009231 ( 0.000010 0.000006 0.000007 ) 0.004516 0.013909 0.009272 ( 0.000006 0.000007 0.000006 ) 0.009231 0.009272 0.018577 ( 0.000007 0.000006 0.000010 ) UB fit with 1033 obs out of 1043 (total:1043,skipped:0) (99.04%) unit cell: 7.379(3) 7.363(2) 7.369(3) 120.24(3) 120.17(4) 89.43(3) V = 282.71(16) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 95 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof 4610 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:02:22 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.161) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) Run 5 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-540.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-588.7455 max=1110576.5297 PROFFIT INFO: background sum: min=-77.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=405.0000 max=5516.0000 PROFFIT INFO: num of signal pixels: min=40 max=488 PROFFIT INFO: Inet: min=-941.9929 max=1776922.3750 PROFFIT INFO: sig(Inet): min=50.3064 max=26825.9570 PROFFIT INFO: Inet/sig(Inet): min=-1.68 max=197.74 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 387 1578 2381 2877 3084 3585 3883 4067 4371 4559 4610 Percent 8.4 34.2 51.6 62.4 66.9 77.8 84.2 88.2 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4610 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 4610 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1776922- 130290 461 405264.39 76.59 100.00 130169- 3895 461 30898.47 19.93 100.00 3884- 2064 461 2839.06 7.08 98.70 2053- 1203 461 1574.44 3.84 50.33 1203- 813 461 992.26 2.29 12.80 813- 551 461 675.63 1.68 7.16 550- 332 461 434.78 1.27 5.64 331- 157 461 243.84 0.71 1.30 157- 20 461 85.30 0.30 0.00 20- -942 461 -123.63 -0.24 0.00 ------------------------------------------------------------------------------------ 1776922- -942 4610 44288.45 11.35 37.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 461 101748.25 16.51 69.63 1.75- 1.28 461 102366.50 22.73 58.57 1.28- 1.08 461 46441.93 13.15 46.85 1.08- 0.93 461 37519.57 12.10 44.47 0.93- 0.84 461 39319.48 11.68 32.32 0.84- 0.76 461 30235.31 9.82 36.01 0.76- 0.69 461 33380.26 10.14 29.72 0.69- 0.63 461 19430.79 6.33 22.13 0.63- 0.57 461 16891.27 5.77 19.96 0.57- 0.44 461 15551.18 5.23 16.27 ------------------------------------------------------------------------------------ 6.55- 0.44 4610 44288.45 11.35 37.59 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:02:22 2019 Sorting 4610 observations 85 unique observations with > 7.00 F2/sig(F2) 4610 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 103 411 5 0 48 460 Total number of frames 460 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 4610 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 17 36 3 0 16 53 4 0 17 71 5 0 8 80 Total number of frames 80 1109 observations > 7.00 F2/sig(F2) 1109 observations in 5 runs Run # start # end # total # 1 0 16 17 2 0 16 34 3 0 16 51 4 0 17 69 5 0 8 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 8.2 (Out of 1109 removed 31 = 1078, unique = 131) 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 1078 observations in 5 runs Run # start # end # total # 1 0 16 17 2 0 16 34 3 0 16 51 4 0 17 69 5 0 8 78 Total number of frames 78 131 unique data precomputed (should be 131) 131 unique data with 1078 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.2 (Out of 1078 removed 0 = 1078, unique = 131) 131 unique data precomputed (should be 131) 131 unique data with 1078 observations RMS deviation of equivalent data = 0.38613 Rint = 0.35370 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.35094, wR= 0.46687 Trying model 1 (ne=2, no=0)... Results: Rint= 0.26988, wR= 0.35047, Acormin=0.511, Acormax=1.464, Acor_av=1.010 F test: Probability=1.000, F= 1.682 Trying model 2 (ne=2, no=1)... Results: Rint= 0.25577, wR= 0.34199, Acormin=0.538, Acormax=1.475, Acor_av=0.990 F test: Probability=0.945, F= 1.110 Trying model 3 (ne=4, no=0)... Results: Rint= 0.26455, wR= 0.34366, Acormin=0.525, Acormax=1.543, Acor_av=0.976 F test: Probability=0.678, F= 1.031 Trying model 4 (ne=4, no=1)... Results: Rint= 0.24467, wR= 0.33025, Acormin=0.456, Acormax=1.591, Acor_av=0.970 F test: Probability=0.997, F= 1.201 Trying model 5 (ne=4, no=3)... Results: Rint= 0.23467, wR= 0.31196, Acormin=0.312, Acormax=1.698, Acor_av=0.911 F test: Probability=0.875, F= 1.079 Trying model 6 (ne=6, no=0)... Results: Rint= 0.26202, wR= 0.32923, Acormin=0.272, Acormax=1.595, Acor_av=0.939 F test: Probability=0.000, F= 0.863 Trying model 7 (ne=6, no=1)... Results: Rint= 0.24243, wR= 0.31068, Acormin=0.282, Acormax=1.720, Acor_av=0.957 F test: Probability=0.526, F= 1.004 Trying model 8 (ne=6, no=3)... Results: Rint= 0.23697, wR= 0.30136, Acormin=0.195, Acormax=1.788, Acor_av=0.884 F test: Probability=0.739, F= 1.043 Trying model 9 (ne=6, no=5)... Results: Rint= 0.23990, wR= 0.30638, Acormin=0.239, Acormax=2.196, Acor_av=0.810 F test: Probability=0.532, F= 1.005 Trying model 10 (ne=8, no=0)... Results: Rint= 0.27939, wR= 0.33225, Acormin=0.050, Acormax=1.629, Acor_av=0.848 F test: Probability=0.000, F= 0.745 Trying model 11 (ne=8, no=1)... Results: Rint= 0.31586, wR= 0.36769, Acormin=0.058, Acormax=1.238, Acor_av=0.648 F test: Probability=0.000, F= 0.581 Trying model 12 (ne=8, no=3)... Results: Rint= 0.33011, wR= 0.37668, Acormin=-0.006, Acormax=0.111, Acor_av=0.040 F test: Probability=0.000, F= 0.527 Trying model 13 (ne=8, no=5)... Results: Rint= 0.31573, wR= 0.36346, Acormin=-0.005, Acormax=0.117, Acor_av=0.041 F test: Probability=0.000, F= 0.569 Trying model 14 (ne=8, no=7)... Results: Rint= 0.24763, wR= 0.30929, Acormin=-0.005, Acormax=0.175, Acor_av=0.044 F test: Probability=0.000, F= 0.910 Final absorption model (ne=4, no=1): Rint= 0.24467, Acormin=0.456, Acormax=1.591, Acor_av=0.970 Combined refinement in use Rint: 0.36755 There are 78 active scales (one needs to be fixed) Refinement control: frame scale #39 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 1 (17 parameters) Refinement control: 94 pars with 4465 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.38613 Using Levenberg-Marquardt: 0.00010 New wR= 0.22908 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35370 with corrections 0.20443 Rint for all data: 0.36755 with corrections 0.21983 0 observations identified as outliers and rejected Cycle 2 wR= 0.22908 Using Levenberg-Marquardt: 0.00001 New wR= 0.21973 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35370 with corrections 0.19344 Rint for all data: 0.36755 with corrections 0.20895 0 observations identified as outliers and rejected Cycle 3 wR= 0.21973 Using Levenberg-Marquardt: 0.00000 New wR= 0.21769 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35370 with corrections 0.19085 Rint for all data: 0.36755 with corrections 0.20637 0 observations identified as outliers and rejected Cycle 4 wR= 0.21769 Using Levenberg-Marquardt: 0.00000 New wR= 0.21825 Using Levenberg-Marquardt: 0.00000 New wR= 0.21825 Using Levenberg-Marquardt: 0.00001 New wR= 0.21825 Using Levenberg-Marquardt: 0.00010 New wR= 0.21821 Using Levenberg-Marquardt: 0.00100 New wR= 0.21793 Using Levenberg-Marquardt: 0.01000 New wR= 0.21720 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35370 with corrections 0.18932 Rint for all data: 0.36755 with corrections 0.20487 0 observations identified as outliers and rejected Cycle 5 wR= 0.21720 Using Levenberg-Marquardt: 0.00100 New wR= 0.21837 Using Levenberg-Marquardt: 0.01000 New wR= 0.21727 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.35370 with corrections 0.18913 Rint for all data: 0.36755 with corrections 0.20467 Final wR= 0.21727 Final frame scales: Min= 0.9399 Max= 3.3875 Final absorption correction factors: Amin= 0.3309 Amax= 1.6466 PROFFIT INFO: Inet (after scale3 abspack): min=-1514.5782 max=1465060.6250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=31.4281 max=31546.6602 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/104 4610 reflections read from tmp file 1151 reflections are rejected (1099 as outliers, 52 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 74 52 37 29 34 19 17 25 145 Initial Chi^2= 2.23473 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.80050 Current error model SIG(F2)^2 = 508.15*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 406.77*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 406.77*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1465061- 124694 461 364244.86 32.43 100.00 124228- 3705 461 27620.85 6.96 83.08 3698- 1953 461 2582.29 2.67 29.28 1945- 1163 461 1514.58 2.04 18.00 1161- 751 461 944.11 1.34 1.08 751- 497 461 618.11 1.17 0.87 496- 304 461 398.90 1.02 0.43 303- 144 461 223.60 0.85 0.65 144- 20 461 77.43 0.52 0.22 20- -1515 461 -144.38 -0.31 0.00 ------------------------------------------------------------------------------------ 1465061- -1515 4610 39808.03 4.87 23.36 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 461 90925.26 11.03 55.10 1.75- 1.28 461 96122.22 9.79 40.35 1.28- 1.08 461 41403.27 5.33 28.85 1.08- 0.93 461 40155.82 4.38 19.96 0.93- 0.84 461 33349.73 4.19 18.00 0.84- 0.76 461 29291.12 3.59 17.14 0.76- 0.69 461 27135.32 3.67 17.57 0.69- 0.63 461 15495.38 2.42 11.50 0.63- 0.57 461 13205.37 2.26 13.23 0.57- 0.44 461 10996.83 2.02 11.93 ------------------------------------------------------------------------------------ 6.55- 0.44 4610 39808.03 4.87 23.36 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 461 90925.26 11.03 55.10 6.55- 1.28 922 93523.74 10.41 47.72 6.55- 1.08 1383 76150.25 8.72 41.43 6.55- 0.93 1844 67151.65 7.64 36.06 6.55- 0.84 2305 60391.26 6.95 32.45 6.55- 0.76 2766 55207.91 6.39 29.90 6.55- 0.69 3227 51197.54 6.00 28.14 6.55- 0.63 3688 46734.77 5.55 26.06 6.55- 0.57 4149 43009.28 5.19 24.63 6.55- 0.44 4610 39808.03 4.87 23.36 ------------------------------------------------------------------------------------ 6.55- 0.44 4610 39808.03 4.87 23.36 Scale applied to data: s=0.682565 (maximum obs:1465060.625,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.205; Rsigma 0.050: data 4610 -> merged 486 With outlier rejection... Rint 0.191; Rsigma 0.051: data 4540 -> merged 486 Rejected total: 70, method kkm 44, method Blessing 26 Completeness direct cell (a, b, c) = (6.563, 6.563, 6.563), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445536, 6.563160 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.35 - 1.59 22 22 25.09 100.00 552 1.55 - 1.22 22 22 23.45 100.00 516 1.20 - 1.02 22 22 21.18 100.00 466 1.02 - 0.92 22 22 16.64 100.00 366 0.92 - 0.84 22 22 16.50 100.00 363 0.84 - 0.79 22 22 13.14 100.00 289 0.79 - 0.75 22 22 12.73 100.00 280 0.75 - 0.71 22 22 10.23 100.00 225 0.71 - 0.69 22 22 10.23 100.00 225 0.68 - 0.65 27 29 9.11 93.10 246 --------------------------------------------------------------- 7.35 - 0.65 225 227 15.68 99.12 3528 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:02:22 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.378599 7.362776 7.368760 120.2407 120.1688 89.4315 4540 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.70 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2264 2277 2281 2270 3411 3010 3017 4540 N (int>3sigma) = 0 255 284 381 259 460 712 713 1047 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 25.1 26.2 26.0 Mean int/sigma = 0.0 1.4 1.5 2.0 1.4 1.6 4.6 4.8 4.7 Lattice type: P chosen Volume: 282.71 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.339 7.355 7.363 119.65 119.84 90.20 Niggli form: a.a = 53.860 b.b = 54.094 c.c = 54.210 b.c = -26.785 a.c = -26.886 a.b = -0.189 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.493 CUBIC F-lattice R(int) = 0.232 [ 4300] Vol = 1130.8 Cell: 10.475 10.408 10.372 89.88 90.12 90.23 Volume: 1130.83 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.427 TETRAGONAL I-lattice R(int) = 0.211 [ 3914] Vol = 565.4 Cell: 7.398 7.369 10.372 90.00 89.83 89.63 Volume: 565.42 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.337 TETRAGONAL I-lattice R(int) = 0.210 [ 3911] Vol = 565.4 Cell: 7.339 7.355 10.475 89.75 90.08 90.20 Volume: 565.42 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.502 TETRAGONAL I-lattice R(int) = 0.211 [ 3914] Vol = 565.4 Cell: 7.369 7.398 10.372 90.17 90.00 90.37 Volume: 565.42 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.360 ORTHORHOMBIC F-lattice R(int) = 0.181 [ 3860] Vol = 1130.8 Cell: 10.372 10.408 10.475 90.23 90.12 89.88 Volume: 1130.83 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.509 ORTHORHOMBIC I-lattice R(int) = 0.168 [ 3837] Vol = 565.4 Cell: 10.372 7.369 7.398 89.63 89.83 90.00 Volume: 565.42 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.326 ORTHORHOMBIC I-lattice R(int) = 0.210 [ 3845] Vol = 565.4 Cell: 7.339 7.355 10.475 90.25 89.92 90.20 Volume: 565.42 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.248 MONOCLINIC I-lattice R(int) = 0.126 [ 3320] Vol = 565.4 Cell: 7.369 10.372 7.398 90.17 90.37 90.00 Volume: 565.42 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.288 MONOCLINIC I-lattice R(int) = 0.173 [ 3320] Vol = 565.4 Cell: 7.363 10.408 7.379 89.75 90.57 90.08 Volume: 565.42 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.248 MONOCLINIC I-lattice R(int) = 0.126 [ 3320] Vol = 565.4 Cell: 7.369 10.372 7.398 90.17 90.37 90.00 Volume: 565.42 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.194 MONOCLINIC I-lattice R(int) = 0.174 [ 3305] Vol = 565.4 Cell: 7.355 7.339 10.475 90.08 90.25 89.80 Volume: 565.42 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.175 MONOCLINIC I-lattice R(int) = 0.180 [ 3326] Vol = 565.4 Cell: 7.339 10.475 7.355 89.75 90.20 90.08 Volume: 565.42 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.288 MONOCLINIC I-lattice R(int) = 0.180 [ 3326] Vol = 565.4 Cell: 7.339 10.475 7.355 90.25 90.20 89.92 Volume: 565.42 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.122 [ 2312] Vol = 282.7 Cell: 7.339 7.355 7.363 119.65 119.84 90.20 Volume: 282.71 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 2281 0 3008 3024 4540 N (int>3sigma) = 0 0 0 0 381 0 718 724 1047 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 26.4 27.1 26.0 Mean int/sigma = 0.0 0.0 0.0 0.0 2.0 0.0 4.7 4.9 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.943 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 28 28 330 886 N I>3s 0 0 0 221 0.0 0.0 -0.0 1.6 0.3 0.3 0.1 2.5 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 0.232 3998 Fd-3m 1 1 227 C N N N N 37 2284 0.231 4064 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.475317 10.408287 10.371891 89.8759 90.1230 90.2286 ZERR 1.00 0.000991 0.011031 0.006070 0.0045 0.0055 0.0946 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 819348- 97204 506 483 48 10.1 336676.87 30.07 0.174 0.188 95897- 2303 612 596 48 12.4 11985.31 4.29 0.295 0.157 2272- 1366 823 816 48 17.0 1869.49 2.11 0.857 0.985 1362- 980 694 685 48 14.3 1119.71 1.34 0.754 0.876 942- 720 469 468 48 9.8 834.96 1.21 0.702 0.723 715- 584 432 426 48 8.9 624.70 0.93 0.726 0.805 577- 449 331 327 48 6.8 479.00 0.85 0.661 0.742 448- 304 323 320 48 6.7 376.96 0.70 0.710 0.839 303- 146 244 243 48 5.1 208.56 0.54 0.809 1.076 128- -456 176 176 54 3.3 25.99 0.14 0.959 3.157 ------------------------------------------------------------------------------------------- 819348- -456 4610 4540 486 9.3 38114.56 4.70 0.191 0.197 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-1.14 1214 1189 49 24.3 72523.64 8.40 0.204 0.232 0.028 1.13-0.89 866 858 48 17.9 40840.51 4.76 0.197 0.206 0.054 0.89-0.76 696 685 49 14.0 33045.50 3.97 0.168 0.193 0.072 0.76-0.69 535 528 50 10.6 23204.48 3.24 0.163 0.180 0.079 0.69-0.63 407 401 48 8.4 17677.13 2.63 0.170 0.148 0.098 0.63-0.59 315 309 50 6.2 10448.55 1.99 0.215 0.227 0.126 0.58-0.55 228 226 48 4.7 16508.13 2.68 0.146 0.144 0.107 0.55-0.52 151 150 49 3.1 5824.72 1.43 0.101 0.100 0.164 0.52-0.49 121 118 49 2.4 13357.81 2.31 0.080 0.083 0.114 0.49-0.45 77 76 46 1.7 5029.97 1.15 0.444 0.527 0.190 ------------------------------------------------------------------------------------------------------ inf-0.45 4610 4540 486 9.3 38114.56 4.70 0.191 0.197 0.051 inf-0.65 3583 3528 225 15.7 45006.51 5.38 0.193 0.211 0.046 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-1.14 1189 49 49 100.0 24.3 72523.64 36.42 0.204 0.007 1.13-0.89 858 48 48 100.0 17.9 40840.51 17.13 0.197 0.018 0.89-0.76 685 49 49 100.0 14.0 33045.50 13.70 0.168 0.023 0.76-0.69 528 50 50 100.0 10.6 23204.48 10.09 0.163 0.028 0.69-0.63 401 50 48 96.0 8.4 17677.13 7.52 0.170 0.046 0.63-0.59 309 56 50 89.3 6.2 10448.55 4.81 0.215 0.055 0.58-0.55 226 55 48 87.3 4.7 16508.13 6.10 0.146 0.051 0.55-0.52 150 66 49 74.2 3.1 5824.72 2.53 0.101 0.088 0.52-0.49 118 83 49 59.0 2.4 13357.81 3.63 0.080 0.073 0.49-0.45 76 145 46 31.7 1.7 5029.97 1.46 0.444 0.891 -------------------------------------------------------------------------------------------- inf-0.45 4540 651 486 74.7 9.3 38114.56 17.51 0.191 0.025 inf-0.65 3528 227 225 99.1 15.7 45006.51 20.98 0.193 0.016 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 No constraint UB - matrix: 0.013199 -0.008942 -0.066336 ( 0.000011 0.000010 0.000010 ) 0.065180 -0.013005 0.014765 ( 0.000011 0.000010 0.000010 ) -0.014521 -0.066303 0.006137 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.004633 -0.000003 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004645 -0.000006 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000006 0.004656 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.013199 -0.008942 -0.066336 ( 0.000011 0.000010 0.000010 ) 0.065180 -0.013005 0.014765 ( 0.000011 0.000010 0.000010 ) -0.014521 -0.066303 0.006137 ( 0.000013 0.000012 0.000011 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4202(17) 10.4070(17) 10.3949(15) 89.929(12) 89.971(13) 89.965(13) V = 1127.3(3) unit cell: 10.4074(5) 10.4074(5) 10.4074(5) 90.0 90.0 90.0 V = 1127.26(9) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.161) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) Run 5 Omega scan: (-6.000 - 44.000,50 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-540.0000 max=7904305.0000 PROFFIT INFO: signal sum lp corr: min=-588.7455 max=1110576.5297 PROFFIT INFO: background sum: min=-77.0000 max=7550.0000 PROFFIT INFO: background sum sig2: min=405.0000 max=5516.0000 PROFFIT INFO: num of signal pixels: min=40 max=488 PROFFIT INFO: Inet: min=-941.9929 max=1776922.3750 PROFFIT INFO: sig(Inet): min=50.3064 max=26825.9570 PROFFIT INFO: Inet/sig(Inet): min=-1.68 max=197.74 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 774 3156 4762 5754 6168 7170 7766 8134 8742 9118 9220 Percent 8.4 34.2 51.6 62.4 66.9 77.8 84.2 88.2 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4610 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 4610 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1776922- 130290 461 405264.39 76.59 100.00 130169- 3895 461 30898.47 19.93 100.00 3884- 2064 461 2839.06 7.08 98.70 2053- 1203 461 1574.44 3.84 50.33 1203- 813 461 992.26 2.29 12.80 813- 551 461 675.63 1.68 7.16 550- 332 461 434.78 1.27 5.64 331- 157 461 243.84 0.71 1.30 157- 20 461 85.30 0.30 0.00 20- -942 461 -123.63 -0.24 0.00 ------------------------------------------------------------------------------------ 1776922- -942 4610 44288.45 11.35 37.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 461 112675.25 15.10 67.90 1.73- 1.26 461 83308.13 21.26 59.87 1.26- 1.09 461 57412.28 18.17 65.94 1.09- 0.96 461 54062.93 15.02 35.14 0.96- 0.88 461 13475.39 6.03 40.78 0.88- 0.81 461 54508.06 15.41 37.96 0.81- 0.76 461 18386.30 5.71 16.92 0.76- 0.71 461 21496.89 7.02 18.22 0.71- 0.67 461 23827.19 7.90 27.55 0.67- 0.63 461 3732.12 1.84 5.64 ------------------------------------------------------------------------------------ 6.00- 0.63 4610 44288.45 11.35 37.59 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:02:23 2019 Sorting 4610 observations 43 unique observations with > 7.00 F2/sig(F2) 4610 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 103 411 5 0 48 460 Total number of frames 460 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 11 frame = 1 scale 4610 observations in 5 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 4 45 Total number of frames 45 1109 observations > 7.00 F2/sig(F2) 1109 observations in 5 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 4 45 Total number of frames 45 Removing 'redundancy=1' reflections Average redundancy: 20.9 (Out of 1109 removed 3 = 1106, unique = 53) 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 1106 observations in 5 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 4 45 Total number of frames 45 53 unique data precomputed (should be 53) 53 unique data with 1106 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.9 (Out of 1106 removed 0 = 1106, unique = 53) 53 unique data precomputed (should be 53) 53 unique data with 1106 observations RMS deviation of equivalent data = 0.25703 Rint = 0.19736 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19323, wR= 0.26986 Trying model 1 (ne=2, no=0)... Results: Rint= 0.10897, wR= 0.16011, Acormin=0.617, Acormax=1.400, Acor_av=1.019 F test: Probability=1.000, F= 3.130 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10032, wR= 0.14787, Acormin=0.494, Acormax=1.466, Acor_av=0.990 F test: Probability=0.996, F= 1.176 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09182, wR= 0.14734, Acormin=0.600, Acormax=1.441, Acor_av=1.006 F test: Probability=0.997, F= 1.187 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08771, wR= 0.13301, Acormin=0.493, Acormax=1.572, Acor_av=0.983 F test: Probability=0.923, F= 1.093 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08252, wR= 0.12416, Acormin=0.574, Acormax=1.675, Acor_av=0.988 F test: Probability=0.999, F= 1.226 Final absorption model (ne=4, no=3): Rint= 0.08252, Acormin=0.574, Acormax=1.675, Acor_av=0.988 Combined refinement in use Rint: 0.19937 There are 45 active scales (one needs to be fixed) Refinement control: frame scale #11 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 68 pars with 2346 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25703 Using Levenberg-Marquardt: 0.00010 New wR= 0.09608 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19736 with corrections 0.07166 Rint for all data: 0.19937 with corrections 0.07450 1 observations identified as outliers and rejected Cycle 2 wR= 0.09260 Using Levenberg-Marquardt: 0.00001 New wR= 0.08429 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19665 with corrections 0.05801 Rint for all data: 0.19937 with corrections 0.06168 1 observations identified as outliers and rejected Cycle 3 wR= 0.07988 Using Levenberg-Marquardt: 0.00000 New wR= 0.08038 Using Levenberg-Marquardt: 0.00001 New wR= 0.08038 Using Levenberg-Marquardt: 0.00010 New wR= 0.08038 Using Levenberg-Marquardt: 0.00100 New wR= 0.08038 Using Levenberg-Marquardt: 0.01000 New wR= 0.08032 Using Levenberg-Marquardt: 0.10000 New wR= 0.08002 Using Levenberg-Marquardt: 1.00000 New wR= 0.07949 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19582 with corrections 0.05508 Rint for all data: 0.19937 with corrections 0.05949 1 observations identified as outliers and rejected Cycle 4 wR= 0.07634 Using Levenberg-Marquardt: 0.10000 New wR= 0.07641 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19542 with corrections 0.05218 Rint for all data: 0.19937 with corrections 0.05720 Final wR= 0.07641 Final frame scales: Min= 0.8568 Max= 1.2162 Final absorption correction factors: Amin= 0.4137 Amax= 1.5142 PROFFIT INFO: Inet (after scale3 abspack): min=-950.9047 max=1256670.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=48.2572 max=24823.8770 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/104 4610 reflections read from tmp file 198 reflections are rejected (198 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 8 0 4 5 4 4 133 Initial Chi^2= 0.51801 Cycle 1, Chi^2= 1.04447 Current error model SIG(F2)^2 = 72.73*I_RAW + 7.75*I_BACK+(0.02810*)^2 Cycle 2, Chi^2= 1.02064 Current error model SIG(F2)^2 = 88.08*I_RAW + 5.20*I_BACK+(0.02310*)^2 Cycle 3, Chi^2= 1.00912 Current error model SIG(F2)^2 = 93.44*I_RAW + 4.26*I_BACK+(0.02253*)^2 Cycle 4, Chi^2= 1.00451 Current error model SIG(F2)^2 = 95.76*I_RAW + 3.84*I_BACK+(0.02242*)^2 Cycle 5, Chi^2= 1.00250 Current error model SIG(F2)^2 = 96.97*I_RAW + 3.62*I_BACK+(0.02236*)^2 Cycle 6, Chi^2= 1.00145 Current error model SIG(F2)^2 = 97.64*I_RAW + 3.49*I_BACK+(0.02233*)^2 Cycle 7, Chi^2= 1.00086 Current error model SIG(F2)^2 = 98.03*I_RAW + 3.42*I_BACK+(0.02231*)^2 Cycle 8, Chi^2= 1.00052 Current error model SIG(F2)^2 = 98.27*I_RAW + 3.38*I_BACK+(0.02229*)^2 Cycle 9, Chi^2= 1.00032 Current error model SIG(F2)^2 = 98.41*I_RAW + 3.35*I_BACK+(0.02229*)^2 Final Chi^2= 1.00032 Final error model SIG(F2)^2 = 98.41*I_RAW + 3.35*I_BACK+(0.02229*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1256670- 120730 461 387242.76 33.46 100.00 120473- 3515 461 30696.26 12.78 100.00 3505- 2043 461 2699.01 5.72 98.92 2040- 1170 461 1540.01 3.77 57.48 1169- 778 461 951.32 2.59 16.70 778- 529 461 647.97 2.28 11.93 528- 328 461 423.36 1.94 8.89 326- 158 461 240.29 1.41 2.17 157- 22 461 85.12 0.80 0.22 21- -951 461 -122.48 -0.53 0.00 ------------------------------------------------------------------------------------ 1256670- -951 4610 42440.36 6.42 39.63 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 461 108165.47 10.60 70.72 1.73- 1.26 461 80286.72 9.87 61.39 1.26- 1.09 461 56474.37 8.43 68.98 1.09- 0.96 461 50986.38 7.02 36.88 0.96- 0.88 461 12696.83 4.30 44.90 0.88- 0.81 461 52566.95 8.36 40.35 0.81- 0.76 461 17365.54 3.81 17.79 0.76- 0.71 461 19672.72 4.85 18.87 0.71- 0.67 461 22538.84 5.28 30.15 0.67- 0.63 461 3649.80 1.71 6.29 ------------------------------------------------------------------------------------ 6.00- 0.63 4610 42440.36 6.42 39.63 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 461 108165.47 10.60 70.72 6.00- 1.26 922 94226.10 10.23 66.05 6.00- 1.09 1383 81642.19 9.63 67.03 6.00- 0.96 1844 73978.24 8.98 59.49 6.00- 0.88 2305 61721.96 8.04 56.57 6.00- 0.81 2766 60196.12 8.09 53.87 6.00- 0.76 3227 54077.47 7.48 48.71 6.00- 0.71 3688 49776.87 7.15 44.98 6.00- 0.67 4149 46750.43 6.94 43.34 6.00- 0.63 4610 42440.36 6.42 39.63 ------------------------------------------------------------------------------------ 6.00- 0.63 4610 42440.36 6.42 39.63 Scale applied to data: s=0.795753 (maximum obs:1256670.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.057; Rsigma 0.035: data 4610 -> merged 162 With outlier rejection... Rint 0.051; Rsigma 0.035: data 4597 -> merged 162 Rejected total: 13, method kkm 5, method Blessing 8 Completeness direct cell (a, b, c) = (10.407, 10.407, 10.407), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626450, 6.008702 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.35 - 1.76 14 14 30.07 100.00 421 1.73 - 1.27 14 14 33.50 100.00 469 1.26 - 1.06 14 14 37.43 100.00 524 1.05 - 0.97 14 14 32.36 100.00 453 0.95 - 0.88 14 14 34.07 100.00 477 0.87 - 0.81 14 14 30.36 100.00 425 0.80 - 0.76 14 14 31.50 100.00 441 0.76 - 0.72 14 14 26.50 100.00 371 0.72 - 0.69 14 14 28.71 100.00 402 0.69 - 0.65 19 19 24.42 100.00 464 --------------------------------------------------------------- 7.35 - 0.65 145 145 30.67 100.00 4447 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:02:22 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.378599 7.362776 7.368760 120.2407 120.1688 89.4315 4540 Reflections read from file xs2212a.hkl; mean (I/sigma) = 4.70 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2264 2277 2281 2270 3411 3010 3017 4540 N (int>3sigma) = 0 255 284 381 259 460 712 713 1047 Mean intensity = 0.0 0.8 0.8 1.2 0.8 0.9 25.1 26.2 26.0 Mean int/sigma = 0.0 1.4 1.5 2.0 1.4 1.6 4.6 4.8 4.7 Lattice type: P chosen Volume: 282.71 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.339 7.355 7.363 119.65 119.84 90.20 Niggli form: a.a = 53.860 b.b = 54.094 c.c = 54.210 b.c = -26.785 a.c = -26.886 a.b = -0.189 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.493 CUBIC F-lattice R(int) = 0.232 [ 4300] Vol = 1130.8 Cell: 10.475 10.408 10.372 89.88 90.12 90.23 Volume: 1130.83 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.427 TETRAGONAL I-lattice R(int) = 0.211 [ 3914] Vol = 565.4 Cell: 7.398 7.369 10.372 90.00 89.83 89.63 Volume: 565.42 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.337 TETRAGONAL I-lattice R(int) = 0.210 [ 3911] Vol = 565.4 Cell: 7.339 7.355 10.475 89.75 90.08 90.20 Volume: 565.42 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.502 TETRAGONAL I-lattice R(int) = 0.211 [ 3914] Vol = 565.4 Cell: 7.369 7.398 10.372 90.17 90.00 90.37 Volume: 565.42 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.360 ORTHORHOMBIC F-lattice R(int) = 0.181 [ 3860] Vol = 1130.8 Cell: 10.372 10.408 10.475 90.23 90.12 89.88 Volume: 1130.83 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.509 ORTHORHOMBIC I-lattice R(int) = 0.168 [ 3837] Vol = 565.4 Cell: 10.372 7.369 7.398 89.63 89.83 90.00 Volume: 565.42 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.326 ORTHORHOMBIC I-lattice R(int) = 0.210 [ 3845] Vol = 565.4 Cell: 7.339 7.355 10.475 90.25 89.92 90.20 Volume: 565.42 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.248 MONOCLINIC I-lattice R(int) = 0.126 [ 3320] Vol = 565.4 Cell: 7.369 10.372 7.398 90.17 90.37 90.00 Volume: 565.42 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.288 MONOCLINIC I-lattice R(int) = 0.173 [ 3320] Vol = 565.4 Cell: 7.363 10.408 7.379 89.75 90.57 90.08 Volume: 565.42 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.248 MONOCLINIC I-lattice R(int) = 0.126 [ 3320] Vol = 565.4 Cell: 7.369 10.372 7.398 90.17 90.37 90.00 Volume: 565.42 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.194 MONOCLINIC I-lattice R(int) = 0.174 [ 3305] Vol = 565.4 Cell: 7.355 7.339 10.475 90.08 90.25 89.80 Volume: 565.42 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.175 MONOCLINIC I-lattice R(int) = 0.180 [ 3326] Vol = 565.4 Cell: 7.339 10.475 7.355 89.75 90.20 90.08 Volume: 565.42 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.288 MONOCLINIC I-lattice R(int) = 0.180 [ 3326] Vol = 565.4 Cell: 7.339 10.475 7.355 90.25 90.20 89.92 Volume: 565.42 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.122 [ 2312] Vol = 282.7 Cell: 7.339 7.355 7.363 119.65 119.84 90.20 Volume: 282.71 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 2281 0 3008 3024 4540 N (int>3sigma) = 0 0 0 0 381 0 718 724 1047 Mean intensity = 0.0 0.0 0.0 0.0 1.2 0.0 26.4 27.1 26.0 Mean int/sigma = 0.0 0.0 0.0 0.0 2.0 0.0 4.7 4.9 4.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.943 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 28 28 330 886 N I>3s 0 0 0 221 0.0 0.0 -0.0 1.6 0.3 0.3 0.1 2.5 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 0.232 3998 Fd-3m 1 1 227 C N N N N 37 2284 0.231 4064 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.475317 10.408287 10.371891 89.8759 90.1230 90.2286 ZERR 1.00 0.000991 0.011031 0.006070 0.0045 0.0055 0.0946 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1150740- 94082 565 556 27 20.6 334286.37 31.01 0.047 0.060 80528- 1829 867 864 27 32.0 5333.94 7.88 0.095 0.126 1718- 777 904 903 27 33.4 1144.73 2.84 0.225 0.295 735- 330 917 917 27 34.0 508.31 1.93 0.378 0.522 326- 67 684 684 27 25.3 218.78 1.16 0.600 1.011 64- -133 673 673 27 24.9 15.16 0.23 0.956 4.240 ------------------------------------------------------------------------------------------- 1150740- -133 4610 4597 162 28.4 41794.95 6.38 0.051 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-1.27 892 888 27 32.9 94627.42 10.39 0.042 0.053 0.026 1.26-0.97 931 928 27 34.4 52914.88 7.61 0.046 0.061 0.032 0.97-0.81 953 951 29 32.8 31576.23 6.18 0.060 0.079 0.042 0.80-0.73 793 792 27 29.3 18039.06 4.24 0.066 0.080 0.055 0.72-0.67 700 699 27 25.9 18746.59 4.53 0.082 0.107 0.063 0.66-0.63 341 339 25 13.6 4653.23 1.89 0.131 0.105 0.116 ------------------------------------------------------------------------------------------------------ inf-0.63 4610 4597 162 28.4 41794.95 6.38 0.051 0.064 0.035 inf-0.65 4456 4445 144 30.9 42977.71 6.53 0.051 0.063 0.035 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-1.27 888 27 27 100.0 32.9 94627.42 56.67 0.042 0.007 1.26-0.97 928 27 27 100.0 34.4 52914.88 42.16 0.046 0.007 0.97-0.81 951 29 29 100.0 32.8 31576.23 35.56 0.060 0.009 0.80-0.73 792 27 27 100.0 29.3 18039.06 20.87 0.066 0.012 0.72-0.67 699 27 27 100.0 25.9 18746.59 24.74 0.082 0.013 0.66-0.63 339 25 25 100.0 13.6 4653.23 7.13 0.131 0.035 -------------------------------------------------------------------------------------------- inf-0.63 4597 162 162 100.0 28.4 41794.95 34.70 0.051 0.009 inf-0.65 4445 144 144 100.0 30.9 42977.71 35.68 0.051 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:08:56 2019) ID: 3668; threads 40; handles 811; mem 515756.00 (1204688.00)kB; time: 1w 5d 0h 19m 44s MEMORY INFO: Memory PF:219.0, Ph:552.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.7,peak PF: 700.2, WS: 471.8, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:221.0, Ph:554.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.5,peak PF: 700.2, WS: 473.6, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:08:56 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000074 0.000063 0.000077 ) 0.064809 0.092374 0.027273 ( 0.000090 0.000077 0.000094 ) 0.045523 0.057900 0.132205 ( 0.000108 0.000092 0.000112 ) 7.38096 ( 0.00603 ) 7.36649 ( 0.00666 ) 7.42630 ( 0.00756 ) 120.52449 ( 0.10257 ) 120.40327 ( 0.09762 ) 89.27095 ( 0.06969 ) V = 283.31 Selected cell (from UM rr/UM ttt/UM f): 14 7.3810 7.3665 7.4263 120.5245 120.4033 89.2710 mI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.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 Wed Aug 21 14:08:56 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.087449 -0.046087 0.017488 ( 0.000074 0.000063 0.000077 ) 0.064809 0.092374 0.027273 ( 0.000090 0.000077 0.000094 ) 0.045523 0.057900 0.132205 ( 0.000108 0.000092 0.000112 ) M - matrix: 0.013768 0.004473 0.009180 ( 0.000020 0.000014 0.000018 ) 0.004473 0.013940 0.009328 ( 0.000014 0.000019 0.000017 ) 0.009180 0.009328 0.018586 ( 0.000018 0.000017 0.000030 ) unit cell: 7.381(6) 7.366(7) 7.426(8) 120.52(10) 120.40(10) 89.27(7) V = 283.3(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) UB - matrix: 0.087241 -0.046051 0.017527 ( 0.000099 0.000066 0.000111 ) 0.064869 0.092387 0.027186 ( 0.000095 0.000063 0.000106 ) 0.045554 0.057903 0.131885 ( 0.000098 0.000065 0.000109 ) M - matrix: 0.013894 0.004613 0.009300 ( 0.000023 0.000014 0.000018 ) 0.004613 0.014009 0.009341 ( 0.000014 0.000015 0.000015 ) 0.009300 0.009341 0.018440 ( 0.000018 0.000015 0.000030 ) unit cell: 7.394(7) 7.365(7) 7.443(7) 120.43(10) 120.42(10) 89.39(8) V = 284.4(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB fit with 198 obs out of 232 (total:232,skipped:0) (85.34%) UB - matrix: 0.087236 -0.046040 0.017577 ( 0.000097 0.000065 0.000109 ) 0.064884 0.092395 0.027224 ( 0.000097 0.000064 0.000108 ) 0.045564 0.057908 0.131894 ( 0.000099 0.000066 0.000111 ) M - matrix: 0.013896 0.004617 0.009309 ( 0.000023 0.000014 0.000019 ) 0.004617 0.014010 0.009344 ( 0.000014 0.000015 0.000016 ) 0.009309 0.009344 0.018446 ( 0.000019 0.000016 0.000030 ) unit cell: 7.396(7) 7.365(7) 7.445(7) 120.43(10) 120.45(10) 89.39(8) V = 284.5(5) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: 0.087242 -0.046020 0.017581 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045653 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013903 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1320 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087242 -0.046020 0.017582 ( 0.000098 0.000065 0.000110 ) 0.064870 0.092341 0.027209 ( 0.000095 0.000063 0.000106 ) 0.045654 0.057830 0.131806 ( 0.000104 0.000069 0.000115 ) M - matrix: 0.013904 0.004615 0.009316 ( 0.000023 0.000014 0.000019 ) 0.004615 0.013989 0.009326 ( 0.000014 0.000015 0.000016 ) 0.009316 0.009326 0.018422 ( 0.000019 0.000016 0.000031 ) UB fit with 199 obs out of 232 (total:232,skipped:0) (85.78%) unit cell: 7.399(7) 7.368(7) 7.452(8) 120.40(10) 120.50(10) 89.38(8) V = 284.9(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 232 (total:232,skipped:0) (89.22%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.61 | 22 | 0.974 ( 0.491) | 0.865 ( 0.195) | 1.502 ( 2.009) | 2.60- 1.76 | 22 | 0.831 ( 0.085) | 0.825 ( 0.144) | 0.775 ( 0.412) | 1.75- 1.57 | 22 | 0.857 ( 0.094) | 0.893 ( 0.147) | 0.674 ( 0.315) | 1.56- 1.35 | 22 | 0.927 ( 0.067) | 0.987 ( 0.120) | 1.013 ( 0.487) | 1.35- 1.16 | 22 | 0.949 ( 0.075) | 1.039 ( 0.133) | 1.020 ( 0.686) | 1.16- 1.01 | 22 | 0.916 ( 0.086) | 0.922 ( 0.169) | 0.949 ( 0.413) | 1.00- 0.88 | 22 | 0.963 ( 0.076) | 0.998 ( 0.118) | 1.194 ( 0.536) | 0.88- 0.79 | 22 | 0.984 ( 0.056) | 1.034 ( 0.144) | 1.153 ( 0.320) | 0.78- 0.69 | 22 | 0.982 ( 0.042) | 0.943 ( 0.104) | 1.275 ( 0.483) | 0.69- 0.63 | 23 | 0.943 ( 0.036) | 0.924 ( 0.093) | 1.313 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 221 | 0.933 ( 0.176) | 0.943 ( 0.155) | 1.088 ( 0.811) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 205 obs out of 221 (total:221,skipped:0) (92.76%) UB - matrix: 0.087423 -0.046183 0.017573 ( 0.000091 0.000059 0.000090 ) 0.064810 0.092235 0.027385 ( 0.000081 0.000052 0.000080 ) 0.045552 0.057573 0.131875 ( 0.000105 0.000068 0.000104 ) M - matrix: 0.013918 0.004563 0.009318 ( 0.000021 0.000013 0.000018 ) 0.004563 0.013955 0.009307 ( 0.000013 0.000014 0.000014 ) 0.009318 0.009307 0.018450 ( 0.000018 0.000014 0.000028 ) unit cell: 7.391(6) 7.372(6) 7.446(7) 120.46(9) 120.58(9) 89.15(7) V = 284.5(4) OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 OTKP changes: 206 1 1 1 UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.000) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087490 -0.046075 0.017427 ( 0.000094 0.000061 0.000091 ) 0.064720 0.092373 0.027219 ( 0.000085 0.000055 0.000082 ) 0.045700 0.057900 0.132175 ( 0.000102 0.000066 0.000099 ) M - matrix: 0.013932 0.004593 0.009327 ( 0.000022 0.000013 0.000017 ) 0.004593 0.014008 0.009364 ( 0.000013 0.000014 0.000014 ) 0.009327 0.009364 0.018515 ( 0.000017 0.000014 0.000027 ) UB fit with 209 obs out of 221 (total:221,skipped:0) (94.57%) unit cell: 7.382(6) 7.367(6) 7.433(7) 120.53(9) 120.46(9) 89.23(7) V = 283.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 221 (total:221,skipped:0) (97.29%) 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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.98 | 21 | 0.996 ( 0.545) | 0.843 ( 0.182) | 1.637 ( 2.376) | 2.60- 1.75 | 21 | 0.826 ( 0.088) | 0.815 ( 0.152) | 0.776 ( 0.329) | 1.75- 1.56 | 21 | 0.858 ( 0.088) | 0.893 ( 0.144) | 0.654 ( 0.193) | 1.56- 1.35 | 21 | 0.955 ( 0.114) | 1.009 ( 0.137) | 1.062 ( 0.543) | 1.35- 1.16 | 21 | 0.967 ( 0.063) | 1.046 ( 0.101) | 0.931 ( 0.372) | 1.16- 1.00 | 21 | 0.938 ( 0.080) | 0.963 ( 0.179) | 0.948 ( 0.409) | 1.00- 0.88 | 21 | 0.965 ( 0.077) | 1.003 ( 0.129) | 1.208 ( 0.515) | 0.88- 0.79 | 21 | 0.980 ( 0.051) | 1.020 ( 0.139) | 1.190 ( 0.362) | 0.78- 0.69 | 21 | 0.980 ( 0.042) | 0.950 ( 0.114) | 1.249 ( 0.471) | 0.69- 0.63 | 23 | 0.950 ( 0.039) | 0.930 ( 0.097) | 1.358 ( 0.480) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 212 | 0.942 ( 0.193) | 0.947 ( 0.158) | 1.104 ( 0.891) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 62 obs out of 277 (total:277,skipped:0) (22.38%) UB - matrix: 0.086668 -0.046652 0.015933 ( 0.000580 0.000355 0.000683 ) 0.062969 0.092062 0.026303 ( 0.000563 0.000344 0.000663 ) 0.046349 0.058433 0.133703 ( 0.000879 0.000537 0.001034 ) M - matrix: 0.013625 0.004462 0.009234 ( 0.000148 0.000090 0.000147 ) 0.004462 0.014066 0.009491 ( 0.000090 0.000095 0.000117 ) 0.009234 0.009491 0.018822 ( 0.000147 0.000117 0.000280 ) unit cell: 7.44(4) 7.36(4) 7.38(6) 120.9(7) 120.4(7) 88.8(5) V = 283(3) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 2, #refl in peak table: 277 #indexed refl 260, indexation with best UB: 93.8628% Lattice: 7.3801 7.3770 7.3526 120.324 120.100 89.502 282.455 Rotation: -23.960 24.230 -35.210 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087673 -0.045037 0.014272 ( 0.000063 0.000075 0.000081 ) 0.061867 0.092802 0.025231 ( 0.000072 0.000086 0.000093 ) 0.048294 0.057128 0.133595 ( 0.000053 0.000064 0.000069 ) M - matrix: 0.013846 0.004552 0.009264 ( 0.000015 0.000012 0.000012 ) 0.004552 0.013904 0.009331 ( 0.000012 0.000019 0.000013 ) 0.009264 0.009331 0.018688 ( 0.000012 0.000013 0.000019 ) unit cell: 7.374(6) 7.377(7) 7.353(5) 120.32(9) 120.07(8) 89.54(7) V = 282.2(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 OTKP changes: 97 1 1 1 UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087597 -0.044978 0.014155 ( 0.000059 0.000071 0.000077 ) 0.061850 0.092873 0.025075 ( 0.000071 0.000085 0.000092 ) 0.048480 0.057055 0.133631 ( 0.000058 0.000069 0.000075 ) M - matrix: 0.013849 0.004570 0.009269 ( 0.000015 0.000012 0.000012 ) 0.004570 0.013904 0.009316 ( 0.000012 0.000019 0.000014 ) 0.009269 0.009316 0.018686 ( 0.000012 0.000014 0.000021 ) UB fit with 260 obs out of 277 (total:277,skipped:0) (93.86%) unit cell: 7.375(5) 7.372(6) 7.346(5) 120.20(9) 120.05(8) 89.68(7) V = 282.1(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 261 obs out of 277 (total:277,skipped:0) (94.22%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.37 | 25 | 0.862 ( 0.090) | 0.867 ( 0.128) | 1.000 ( 0.479) | 2.37- 1.75 | 25 | 0.875 ( 0.104) | 0.882 ( 0.156) | 1.038 ( 0.554) | 1.75- 1.58 | 25 | 0.907 ( 0.085) | 0.891 ( 0.139) | 0.968 ( 0.392) | 1.58- 1.35 | 25 | 0.936 ( 0.081) | 0.967 ( 0.111) | 0.858 ( 0.385) | 1.35- 1.19 | 25 | 0.918 ( 0.077) | 0.915 ( 0.112) | 1.009 ( 0.629) | 1.19- 1.09 | 25 | 0.927 ( 0.063) | 0.964 ( 0.119) | 0.833 ( 0.331) | 1.09- 0.92 | 25 | 0.954 ( 0.070) | 0.981 ( 0.099) | 1.047 ( 0.418) | 0.91- 0.86 | 25 | 0.937 ( 0.069) | 0.936 ( 0.100) | 1.044 ( 0.367) | 0.86- 0.73 | 25 | 0.949 ( 0.055) | 0.901 ( 0.086) | 1.394 ( 0.455) | 0.73- 0.63 | 28 | 0.932 ( 0.034) | 0.886 ( 0.092) | 1.326 ( 0.468) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 253 | 0.920 ( 0.080) | 0.919 ( 0.122) | 1.055 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.087514 -0.045148 0.014042 ( 0.000043 0.000052 0.000055 ) 0.061984 0.093199 0.025298 ( 0.000037 0.000046 0.000048 ) 0.048733 0.057069 0.133851 ( 0.000041 0.000050 0.000053 ) M - matrix: 0.013876 0.004607 0.009320 ( 0.000010 0.000008 0.000008 ) 0.004607 0.013981 0.009363 ( 0.000008 0.000011 0.000009 ) 0.009320 0.009363 0.018753 ( 0.000008 0.000009 0.000015 ) unit cell: 7.377(4) 7.352(4) 7.340(4) 120.17(5) 120.13(5) 89.72(4) V = 280.9(2) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087515 -0.045162 0.014029 ( 0.000045 0.000056 0.000059 ) 0.062006 0.093009 0.025380 ( 0.000037 0.000045 0.000047 ) 0.048469 0.057047 0.133649 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013853 0.004580 0.009279 ( 0.000010 0.000007 0.000007 ) 0.004580 0.013945 0.009351 ( 0.000007 0.000011 0.000007 ) 0.009279 0.009351 0.018703 ( 0.000007 0.000007 0.000011 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 7.375(4) 7.368(4) 7.351(3) 120.29(5) 120.07(5) 89.63(4) V = 281.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) 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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.38 | 25 | 0.868 ( 0.089) | 0.868 ( 0.127) | 1.025 ( 0.497) | 2.38- 1.76 | 25 | 0.878 ( 0.098) | 0.890 ( 0.140) | 0.975 ( 0.518) | 1.75- 1.58 | 25 | 0.898 ( 0.093) | 0.894 ( 0.154) | 0.966 ( 0.424) | 1.58- 1.35 | 25 | 0.954 ( 0.069) | 0.975 ( 0.102) | 0.873 ( 0.449) | 1.35- 1.19 | 25 | 0.914 ( 0.063) | 0.907 ( 0.112) | 1.003 ( 0.610) | 1.19- 1.09 | 25 | 0.937 ( 0.063) | 0.982 ( 0.090) | 0.845 ( 0.280) | 1.09- 0.92 | 25 | 0.961 ( 0.070) | 0.985 ( 0.097) | 1.119 ( 0.464) | 0.92- 0.87 | 25 | 0.944 ( 0.068) | 0.938 ( 0.092) | 1.030 ( 0.382) | 0.86- 0.73 | 25 | 0.955 ( 0.052) | 0.916 ( 0.086) | 1.299 ( 0.449) | 0.73- 0.63 | 29 | 0.929 ( 0.038) | 0.880 ( 0.094) | 1.341 ( 0.462) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 254 | 0.924 ( 0.078) | 0.923 ( 0.119) | 1.052 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 57 obs out of 253 (total:253,skipped:0) (22.53%) UB - matrix: 0.086857 -0.045149 0.014965 ( 0.000181 0.000235 0.000443 ) 0.064735 0.092733 0.027280 ( 0.000147 0.000191 0.000360 ) 0.045454 0.058254 0.131670 ( 0.000170 0.000222 0.000417 ) M - matrix: 0.013801 0.004729 0.009051 ( 0.000040 0.000032 0.000054 ) 0.004729 0.014031 0.009524 ( 0.000032 0.000049 0.000055 ) 0.009051 0.009524 0.018305 ( 0.000054 0.000055 0.000112 ) unit cell: 7.345(18) 7.45(2) 7.46(3) 121.2(3) 119.1(3) 90.1(2) V = 287(1) OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 OTKP changes: 54 1 1 1 UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087822 -0.044330 0.013027 ( 0.000063 0.000058 0.000073 ) 0.061751 0.094110 0.026069 ( 0.000045 0.000042 0.000052 ) 0.048776 0.055868 0.133075 ( 0.000065 0.000060 0.000075 ) M - matrix: 0.013905 0.004643 0.009245 ( 0.000014 0.000009 0.000012 ) 0.004643 0.013943 0.009310 ( 0.000009 0.000012 0.000011 ) 0.009245 0.009310 0.018558 ( 0.000012 0.000011 0.000020 ) UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) unit cell: 7.355(5) 7.366(4) 7.360(5) 120.12(6) 119.84(7) 90.03(5) V = 282.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 237 obs out of 253 (total:253,skipped:0) (93.68%) 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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 236 peaks identified as outliers and rejected 236 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 236 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 236 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 2.38 | 24 | 0.860 ( 0.097) | 0.876 ( 0.142) | 1.236 ( 0.741) | 2.37- 1.75 | 24 | 0.898 ( 0.098) | 0.913 ( 0.147) | 1.032 ( 0.569) | 1.75- 1.58 | 24 | 0.919 ( 0.086) | 0.955 ( 0.126) | 0.775 ( 0.281) | 1.58- 1.35 | 24 | 0.946 ( 0.077) | 0.962 ( 0.141) | 0.927 ( 0.383) | 1.35- 1.19 | 24 | 0.968 ( 0.062) | 0.999 ( 0.113) | 0.932 ( 0.484) | 1.16- 1.00 | 24 | 0.979 ( 0.058) | 1.024 ( 0.086) | 0.971 ( 0.428) | 1.00- 0.88 | 24 | 0.976 ( 0.103) | 0.988 ( 0.119) | 1.016 ( 0.422) | 0.88- 0.79 | 24 | 1.006 ( 0.045) | 0.994 ( 0.121) | 0.988 ( 0.411) | 0.78- 0.69 | 24 | 0.997 ( 0.043) | 0.988 ( 0.127) | 1.268 ( 0.467) | 0.69- 0.63 | 20 | 0.975 ( 0.055) | 0.907 ( 0.115) | 1.245 ( 0.491) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.88- 0.63 | 236 | 0.952 ( 0.088) | 0.961 ( 0.133) | 1.035 ( 0.505) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) UB - matrix: 0.087928 -0.044332 0.012992 ( 0.000033 0.000032 0.000038 ) 0.061808 0.094168 0.026114 ( 0.000021 0.000020 0.000024 ) 0.048829 0.055684 0.133266 ( 0.000035 0.000034 0.000040 ) M - matrix: 0.013936 0.004641 0.009264 ( 0.000007 0.000005 0.000006 ) 0.004641 0.013934 0.009304 ( 0.000005 0.000006 0.000006 ) 0.009264 0.009304 0.018611 ( 0.000006 0.000006 0.000011 ) unit cell: 7.345(2) 7.362(2) 7.343(2) 120.05(3) 119.83(3) 90.06(2) V = 281.16(15) OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 OTKP changes: 236 1 1 1 UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1288 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087790 -0.044289 0.013047 ( 0.000032 0.000031 0.000036 ) 0.061845 0.094162 0.026140 ( 0.000022 0.000021 0.000025 ) 0.048855 0.055794 0.133156 ( 0.000025 0.000024 0.000028 ) M - matrix: 0.013919 0.004661 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004661 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018584 ( 0.000005 0.000005 0.000008 ) UB fit with 236 obs out of 236 (total:236,skipped:0) (100.00%) unit cell: 7.356(2) 7.365(2) 7.3554(19) 120.06(3) 119.85(3) 90.11(2) V = 281.91(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 236 obs out of 236 (total:236,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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.875 ( 0.089) | 0.896 ( 0.124) | 1.167 ( 0.674) | 2.37- 1.76 | 24 | 0.888 ( 0.109) | 0.897 ( 0.167) | 1.033 ( 0.558) | 1.75- 1.58 | 24 | 0.904 ( 0.087) | 0.940 ( 0.134) | 0.760 ( 0.331) | 1.58- 1.35 | 24 | 0.963 ( 0.068) | 1.004 ( 0.106) | 0.980 ( 0.507) | 1.35- 1.19 | 24 | 0.948 ( 0.070) | 0.956 ( 0.143) | 0.946 ( 0.507) | 1.19- 1.06 | 24 | 0.976 ( 0.066) | 0.999 ( 0.120) | 0.917 ( 0.423) | 1.06- 0.89 | 24 | 0.972 ( 0.058) | 0.990 ( 0.100) | 1.103 ( 0.504) | 0.88- 0.82 | 24 | 1.005 ( 0.047) | 1.008 ( 0.130) | 0.907 ( 0.354) | 0.79- 0.69 | 24 | 0.998 ( 0.044) | 1.006 ( 0.137) | 1.289 ( 0.497) | 0.69- 0.63 | 23 | 0.979 ( 0.051) | 0.913 ( 0.103) | 1.157 ( 0.432) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.951 ( 0.084) | 0.961 ( 0.136) | 1.025 ( 0.510) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 46 obs out of 238 (total:238,skipped:0) (19.33%) UB - matrix: 0.086322 -0.045974 0.017116 ( 0.000473 0.000165 0.000229 ) 0.064318 0.092941 0.027760 ( 0.000633 0.000220 0.000306 ) 0.045617 0.058321 0.132889 ( 0.000830 0.000289 0.000401 ) M - matrix: 0.013669 0.004670 0.009325 ( 0.000138 0.000083 0.000117 ) 0.004670 0.014153 0.009543 ( 0.000083 0.000055 0.000055 ) 0.009325 0.009543 0.018723 ( 0.000117 0.000055 0.000108 ) unit cell: 7.47(3) 7.36(3) 7.42(3) 120.7(5) 120.4(5) 89.5(4) V = 285(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 4, #refl in peak table: 238 #indexed refl 216, indexation with best UB: 90.7563% Lattice: 7.4072 7.3556 7.3610 120.005 120.354 89.764 282.632 Rotation: -22.660 24.759 -35.022 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 227 obs out of 238 (total:238,skipped:0) (95.38%) UB - matrix: 0.087760 -0.044390 0.012681 ( 0.000052 0.000055 0.000059 ) 0.061495 0.094382 0.026268 ( 0.000060 0.000065 0.000069 ) 0.049386 0.055440 0.133261 ( 0.000059 0.000063 0.000067 ) M - matrix: 0.013922 0.004646 0.009310 ( 0.000013 0.000010 0.000011 ) 0.004646 0.013952 0.009304 ( 0.000010 0.000015 0.000012 ) 0.009310 0.009304 0.018609 ( 0.000011 0.000012 0.000018 ) unit cell: 7.369(4) 7.355(5) 7.360(5) 120.01(7) 120.09(6) 89.95(5) V = 281.8(3) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1316 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087844 -0.044328 0.012584 ( 0.000050 0.000054 0.000058 ) 0.061491 0.094437 0.026170 ( 0.000059 0.000063 0.000068 ) 0.049402 0.055462 0.133146 ( 0.000054 0.000058 0.000062 ) M - matrix: 0.013938 0.004653 0.009292 ( 0.000013 0.000009 0.000010 ) 0.004653 0.013959 0.009298 ( 0.000009 0.000014 0.000011 ) 0.009292 0.009298 0.018571 ( 0.000010 0.000011 0.000017 ) UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) unit cell: 7.360(4) 7.354(5) 7.362(4) 120.00(7) 120.01(6) 90.00(5) V = 281.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 231 obs out of 238 (total:238,skipped:0) (97.06%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 223 peaks identified as outliers and rejected 223 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 223 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 223 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 2.38 | 22 | 0.899 ( 0.094) | 0.905 ( 0.131) | 0.958 ( 0.493) | 2.38- 1.83 | 22 | 0.900 ( 0.110) | 0.921 ( 0.154) | 0.939 ( 0.269) | 1.76- 1.58 | 22 | 0.887 ( 0.115) | 0.904 ( 0.161) | 0.806 ( 0.264) | 1.58- 1.35 | 22 | 0.954 ( 0.082) | 0.983 ( 0.130) | 0.791 ( 0.395) | 1.35- 1.19 | 22 | 0.935 ( 0.082) | 0.954 ( 0.100) | 0.903 ( 0.428) | 1.19- 1.00 | 22 | 0.962 ( 0.087) | 0.981 ( 0.123) | 0.884 ( 0.304) | 1.00- 0.88 | 22 | 0.988 ( 0.064) | 0.995 ( 0.081) | 1.052 ( 0.398) | 0.88- 0.79 | 22 | 0.993 ( 0.048) | 0.994 ( 0.129) | 0.938 ( 0.310) | 0.79- 0.69 | 22 | 0.975 ( 0.044) | 0.932 ( 0.088) | 1.196 ( 0.465) | 0.69- 0.63 | 25 | 0.933 ( 0.047) | 0.852 ( 0.068) | 1.275 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.96- 0.63 | 223 | 0.942 ( 0.089) | 0.941 ( 0.128) | 0.978 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) UB - matrix: 0.088106 -0.044293 0.012828 ( 0.000028 0.000032 0.000033 ) 0.061394 0.094519 0.026063 ( 0.000022 0.000026 0.000027 ) 0.049283 0.055378 0.133130 ( 0.000021 0.000024 0.000025 ) M - matrix: 0.013961 0.004630 0.009291 ( 0.000006 0.000004 0.000005 ) 0.004630 0.013962 0.009268 ( 0.000004 0.000006 0.000005 ) 0.009291 0.009268 0.018567 ( 0.000005 0.000005 0.000007 ) unit cell: 7.351(2) 7.341(2) 7.3536(18) 119.91(3) 120.04(3) 89.95(2) V = 280.88(13) OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 UB - matrix: 0.087896 -0.044356 0.012683 ( 0.000021 0.000024 0.000025 ) 0.061495 0.094417 0.026185 ( 0.000020 0.000022 0.000024 ) 0.049387 0.055447 0.133218 ( 0.000019 0.000022 0.000023 ) M - matrix: 0.013946 0.004646 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013956 0.009296 ( 0.000004 0.000005 0.000004 ) 0.009304 0.009296 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3589(17) 7.3517(18) 7.3584(16) 119.99(2) 120.05(2) 89.96(2) V = 281.42(11) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087896 -0.044356 0.012683 ( 0.000021 0.000024 0.000025 ) 0.061495 0.094417 0.026185 ( 0.000020 0.000022 0.000024 ) 0.049387 0.055447 0.133218 ( 0.000019 0.000022 0.000023 ) M - matrix: 0.013946 0.004646 0.009304 ( 0.000005 0.000004 0.000004 ) 0.004646 0.013956 0.009296 ( 0.000004 0.000005 0.000004 ) 0.009304 0.009296 0.018594 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3589(17) 7.3517(18) 7.3584(16) 119.99(2) 120.05(2) 89.96(2) V = 281.42(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) 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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 223 peaks identified as outliers and rejected 223 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 223 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 223 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 22 | 0.868 ( 0.103) | 0.880 ( 0.128) | 0.911 ( 0.399) | 2.38- 1.83 | 22 | 0.907 ( 0.104) | 0.924 ( 0.157) | 0.918 ( 0.259) | 1.76- 1.59 | 22 | 0.880 ( 0.117) | 0.891 ( 0.164) | 0.729 ( 0.225) | 1.58- 1.45 | 22 | 0.947 ( 0.083) | 0.969 ( 0.129) | 0.883 ( 0.461) | 1.45- 1.19 | 22 | 0.926 ( 0.075) | 0.944 ( 0.084) | 0.839 ( 0.422) | 1.19- 1.06 | 22 | 0.980 ( 0.083) | 1.000 ( 0.124) | 0.894 ( 0.363) | 1.01- 0.88 | 22 | 0.983 ( 0.064) | 1.014 ( 0.078) | 1.039 ( 0.371) | 0.88- 0.79 | 22 | 0.991 ( 0.048) | 0.987 ( 0.128) | 0.966 ( 0.330) | 0.79- 0.69 | 22 | 0.976 ( 0.044) | 0.935 ( 0.090) | 1.283 ( 0.490) | 0.69- 0.63 | 25 | 0.933 ( 0.048) | 0.854 ( 0.073) | 1.273 ( 0.428) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 223 | 0.939 ( 0.090) | 0.939 ( 0.130) | 0.977 ( 0.421) | 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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb PROFFITPEAK info: 373 peaks in the peak location table UB fit with 56 obs out of 206 (total:207,skipped:1) (27.18%) UB - matrix: 0.087406 -0.046737 0.017195 ( 0.000176 0.000567 0.000196 ) 0.064427 0.092280 0.027298 ( 0.000190 0.000611 0.000212 ) 0.045746 0.058984 0.132558 ( 0.000252 0.000811 0.000281 ) M - matrix: 0.013883 0.004559 0.009326 ( 0.000046 0.000077 0.000042 ) 0.004559 0.014179 0.009534 ( 0.000077 0.000157 0.000113 ) 0.009326 0.009534 0.018612 ( 0.000042 0.000113 0.000076 ) unit cell: 7.39(3) 7.36(4) 7.46(3) 121.1(5) 120.6(5) 88.6(4) V = 283(2) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 5, #refl in peak table: 207 #indexed refl 188, indexation with best UB: 90.7767% Lattice: 7.3563 7.3400 7.3453 119.932 120.115 89.777 280.788 Rotation: -22.592 24.677 -34.950 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 193 obs out of 206 (total:207,skipped:1) (93.69%) UB - matrix: 0.087887 -0.044569 0.012438 ( 0.000049 0.000064 0.000054 ) 0.061417 0.094424 0.026071 ( 0.000052 0.000068 0.000056 ) 0.049285 0.055191 0.133166 ( 0.000044 0.000057 0.000048 ) M - matrix: 0.013925 0.004602 0.009257 ( 0.000012 0.000010 0.000009 ) 0.004602 0.013948 0.009257 ( 0.000010 0.000015 0.000010 ) 0.009257 0.009257 0.018568 ( 0.000009 0.000010 0.000013 ) unit cell: 7.351(4) 7.342(5) 7.346(4) 119.93(6) 119.98(6) 89.92(5) V = 280.9(3) OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 UB fit with 193 obs out of 206 (total:207,skipped:1) (93.69%) UB - matrix: 0.087890 -0.044568 0.012432 ( 0.000049 0.000064 0.000053 ) 0.061418 0.094425 0.026067 ( 0.000052 0.000068 0.000057 ) 0.049286 0.055191 0.133162 ( 0.000044 0.000058 0.000048 ) M - matrix: 0.013926 0.004603 0.009257 ( 0.000012 0.000010 0.000009 ) 0.004603 0.013948 0.009257 ( 0.000010 0.000015 0.000010 ) 0.009257 0.009257 0.018566 ( 0.000009 0.000010 0.000013 ) unit cell: 7.351(4) 7.342(5) 7.346(4) 119.93(6) 119.97(6) 89.92(5) V = 280.9(3) OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 OTKP changes: 72 1 1 1 207 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Run 5 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 1003 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087890 -0.044568 0.012432 ( 0.000049 0.000064 0.000053 ) 0.061418 0.094425 0.026067 ( 0.000052 0.000068 0.000057 ) 0.049286 0.055191 0.133161 ( 0.000044 0.000058 0.000048 ) M - matrix: 0.013926 0.004603 0.009257 ( 0.000012 0.000010 0.000009 ) 0.004603 0.013948 0.009257 ( 0.000010 0.000015 0.000010 ) 0.009257 0.009257 0.018566 ( 0.000009 0.000010 0.000013 ) UB fit with 193 obs out of 206 (total:207,skipped:1) (93.69%) unit cell: 7.351(4) 7.342(5) 7.346(4) 119.93(6) 119.97(6) 89.92(5) V = 280.9(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 194 obs out of 206 (total:207,skipped:1) (94.17%) 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= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb 0 of 188 peaks identified as outliers and rejected 188 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 188 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 188 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.95- 2.36 | 19 | 0.896 ( 0.108) | 0.900 ( 0.137) | 0.857 ( 0.206) | 2.13- 1.75 | 19 | 0.899 ( 0.129) | 1.021 ( 0.426) | 0.978 ( 0.675) | 1.75- 1.57 | 19 | 0.942 ( 0.125) | 0.944 ( 0.154) | 0.916 ( 0.334) | 1.56- 1.35 | 19 | 0.978 ( 0.092) | 0.988 ( 0.133) | 0.878 ( 0.365) | 1.35- 1.19 | 19 | 0.963 ( 0.097) | 0.997 ( 0.171) | 0.755 ( 0.200) | 1.19- 1.06 | 19 | 1.005 ( 0.058) | 1.039 ( 0.115) | 0.908 ( 0.269) | 1.06- 0.91 | 19 | 1.012 ( 0.075) | 1.065 ( 0.124) | 0.883 ( 0.303) | 0.89- 0.86 | 19 | 1.014 ( 0.067) | 1.025 ( 0.123) | 1.025 ( 0.274) | 0.85- 0.73 | 19 | 1.057 ( 0.047) | 1.003 ( 0.126) | 1.075 ( 0.398) | 0.72- 0.63 | 17 | 1.013 ( 0.044) | 1.060 ( 0.141) | 1.092 ( 0.372) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.95- 0.63 | 188 | 0.978 ( 0.103) | 1.004 ( 0.194) | 0.935 ( 0.376) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 188 obs out of 188 (total:188,skipped:0) (100.00%) UB - matrix: 0.088049 -0.044409 0.012660 ( 0.000025 0.000028 0.000027 ) 0.061615 0.094627 0.026398 ( 0.000035 0.000038 0.000038 ) 0.049425 0.055198 0.133231 ( 0.000024 0.000027 0.000026 ) M - matrix: 0.013992 0.004648 0.009326 ( 0.000007 0.000005 0.000005 ) 0.004648 0.013973 0.009290 ( 0.000005 0.000008 0.000005 ) 0.009326 0.009290 0.018608 ( 0.000005 0.000005 0.000007 ) unit cell: 7.348(2) 7.341(3) 7.352(2) 119.93(3) 120.09(3) 89.95(3) V = 280.50(16) OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 UB - matrix: 0.087884 -0.044471 0.012527 ( 0.000024 0.000027 0.000027 ) 0.061555 0.094488 0.026285 ( 0.000031 0.000034 0.000034 ) 0.049396 0.055210 0.133227 ( 0.000023 0.000026 0.000025 ) M - matrix: 0.013953 0.004635 0.009300 ( 0.000006 0.000005 0.000005 ) 0.004635 0.013954 0.009282 ( 0.000005 0.000007 0.000005 ) 0.009300 0.009282 0.018597 ( 0.000005 0.000005 0.000007 ) UB fit with 188 obs out of 188 (total:188,skipped:0) (100.00%) unit cell: 7.354(2) 7.347(3) 7.351(2) 119.94(3) 120.04(3) 89.96(3) V = 281.02(15) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 1004 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087884 -0.044471 0.012527 ( 0.000024 0.000027 0.000027 ) 0.061555 0.094488 0.026285 ( 0.000031 0.000034 0.000034 ) 0.049396 0.055210 0.133227 ( 0.000023 0.000026 0.000025 ) M - matrix: 0.013953 0.004635 0.009300 ( 0.000006 0.000005 0.000005 ) 0.004635 0.013954 0.009282 ( 0.000005 0.000007 0.000005 ) 0.009300 0.009282 0.018597 ( 0.000005 0.000005 0.000007 ) UB fit with 188 obs out of 188 (total:188,skipped:0) (100.00%) unit cell: 7.354(2) 7.347(3) 7.351(2) 119.94(3) 120.04(3) 89.96(3) V = 281.02(15) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 188 obs out of 188 (total:188,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= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb 0 of 192 peaks identified as outliers and rejected 192 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 192 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 192 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 19 | 0.901 ( 0.106) | 0.917 ( 0.145) | 0.816 ( 0.159) | 2.12- 1.75 | 19 | 0.907 ( 0.138) | 1.000 ( 0.311) | 0.954 ( 0.485) | 1.75- 1.56 | 19 | 0.940 ( 0.129) | 0.943 ( 0.161) | 0.909 ( 0.349) | 1.56- 1.35 | 19 | 0.999 ( 0.076) | 1.027 ( 0.116) | 0.815 ( 0.341) | 1.35- 1.19 | 19 | 0.928 ( 0.109) | 0.951 ( 0.163) | 0.704 ( 0.283) | 1.19- 1.09 | 19 | 0.990 ( 0.059) | 0.988 ( 0.148) | 0.904 ( 0.276) | 1.06- 0.97 | 19 | 1.016 ( 0.075) | 1.076 ( 0.128) | 0.858 ( 0.266) | 0.97- 0.87 | 19 | 1.016 ( 0.071) | 1.017 ( 0.114) | 1.089 ( 0.388) | 0.87- 0.73 | 19 | 1.052 ( 0.058) | 1.017 ( 0.129) | 1.061 ( 0.354) | 0.73- 0.63 | 21 | 1.015 ( 0.041) | 1.034 ( 0.131) | 1.093 ( 0.395) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 192 | 0.977 ( 0.104) | 0.997 ( 0.170) | 0.922 ( 0.363) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.1 | 112 | 0.992 ( 0.040) | 1.036 ( 0.066) | 1.090 ( 0.462) | 10.1-14.9 | 112 | 0.992 ( 0.047) | 1.046 ( 0.071) | 1.141 ( 0.512) | 14.9-18.9 | 112 | 0.997 ( 0.200) | 1.031 ( 0.100) | 1.151 ( 1.044) | 18.9-23.5 | 112 | 0.968 ( 0.058) | 1.008 ( 0.082) | 0.922 ( 0.401) | 23.5-27.1 | 112 | 0.969 ( 0.063) | 1.004 ( 0.096) | 0.954 ( 0.420) | 27.1-32.4 | 112 | 0.952 ( 0.087) | 0.967 ( 0.114) | 0.938 ( 0.440) | 32.5-36.4 | 112 | 0.922 ( 0.155) | 0.901 ( 0.132) | 1.049 ( 0.618) | 36.4-39.0 | 112 | 0.887 ( 0.100) | 0.873 ( 0.183) | 1.005 ( 0.490) | 39.0-42.0 | 112 | 0.905 ( 0.097) | 0.855 ( 0.131) | 1.032 ( 0.462) | 42.0-50.1 | 112 | 0.866 ( 0.122) | 0.793 ( 0.139) | 0.907 ( 0.454) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1120 | 0.945 ( 0.117) | 0.951 ( 0.144) | 1.019 ( 0.567) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.14 e2 dimension: a=-0.0068 b=1.24 e3 dimension: a=0.0008 b=1.08 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 5521 lp-corr: 3814 Maximum peak integral for reflections I/sig<= 100 - raw: 460596 lp-corr: 386392 Maximum peak integral for reflections I/sig<= 10000 - raw: 9692377 lp-corr: 1568264 PROFFITPEAK - Finished at Wed Aug 21 14:09:12 2019 PROFFITMAIN - Started at Wed Aug 21 14:09:12 2019 OTKP changes: 401 2 4 5 OTKP changes: 401 2 4 5 OTKP changes: 401 2 4 5 UB - matrix: 0.087809 -0.045978 0.016573 ( 0.000066 0.000061 0.000073 ) 0.062878 0.092300 0.026701 ( 0.000075 0.000069 0.000082 ) 0.045473 0.057627 0.132089 ( 0.000084 0.000077 0.000092 ) M - matrix: 0.013732 0.004387 0.009141 ( 0.000017 0.000012 0.000015 ) 0.004387 0.013954 0.009314 ( 0.000012 0.000016 0.000014 ) 0.009141 0.009314 0.018435 ( 0.000015 0.000014 0.000025 ) UB fit with 484 obs out of 1120 (total:1120,skipped:0) (43.21%) unit cell: 7.397(5) 7.378(6) 7.438(6) 120.90(9) 120.38(8) 88.56(6) V = 285.0(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= -24.44 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 190 obs out of 212 (total:212,skipped:0) (89.62%) UB - matrix: 0.087751 -0.046099 0.017304 ( 0.000103 0.000063 0.000101 ) 0.064321 0.092328 0.027102 ( 0.000102 0.000062 0.000100 ) 0.045679 0.057683 0.132000 ( 0.000123 0.000075 0.000121 ) M - matrix: 0.013924 0.004528 0.009291 ( 0.000025 0.000015 0.000021 ) 0.004528 0.013977 0.009319 ( 0.000015 0.000016 0.000016 ) 0.009291 0.009319 0.018458 ( 0.000021 0.000016 0.000033 ) unit cell: 7.377(7) 7.367(7) 7.441(8) 120.57(11) 120.52(11) 88.99(8) V = 283.7(5) OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 OTKP changes: 203 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.165) HKL list info: 1291 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087503 -0.046201 0.017335 ( 0.000101 0.000063 0.000094 ) 0.064812 0.092373 0.027276 ( 0.000084 0.000052 0.000078 ) 0.045761 0.057808 0.132111 ( 0.000106 0.000066 0.000098 ) M - matrix: 0.013952 0.004589 0.009330 ( 0.000023 0.000013 0.000018 ) 0.004589 0.014009 0.009356 ( 0.000013 0.000014 0.000013 ) 0.009330 0.009356 0.018498 ( 0.000018 0.000013 0.000026 ) UB fit with 200 obs out of 212 (total:212,skipped:0) (94.34%) unit cell: 7.378(7) 7.365(6) 7.437(6) 120.52(9) 120.49(9) 89.20(7) V = 283.3(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 212 (total:212,skipped:0) (96.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* UB - matrix: 0.117983 0.039019 0.078678 ( 0.000074 0.000046 0.000068 ) 0.000077 0.111557 0.056265 ( 0.000080 0.000050 0.000074 ) -0.000079 -0.000069 0.095367 ( 0.000089 0.000055 0.000082 ) M - matrix: 0.013920 0.004612 0.009279 ( 0.000017 0.000011 0.000014 ) 0.004612 0.013967 0.009340 ( 0.000011 0.000012 0.000011 ) 0.009279 0.009340 0.018451 ( 0.000014 0.000011 0.000021 ) UB fit with 206 obs out of 212 (total:212,skipped:0) (97.17%) unit cell: 7.374(5) 7.380(5) 7.432(8) 120.48(9) 120.24(9) 89.47(6) V = 284.1(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.44 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.32 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.087486 -0.045184 0.014006 ( 0.000045 0.000055 0.000058 ) 0.062041 0.093036 0.025395 ( 0.000037 0.000045 0.000047 ) 0.048470 0.057052 0.133667 ( 0.000030 0.000037 0.000038 ) M - matrix: 0.013852 0.004584 0.009280 ( 0.000010 0.000007 0.000007 ) 0.004584 0.013952 0.009356 ( 0.000007 0.000011 0.000008 ) 0.009280 0.009356 0.018708 ( 0.000007 0.000008 0.000011 ) unit cell: 7.375(4) 7.366(4) 7.349(3) 120.28(5) 120.06(5) 89.65(4) V = 281.7(2) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) HKL list info: 1305 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087471 -0.045179 0.013989 ( 0.000045 0.000055 0.000058 ) 0.062038 0.093009 0.025387 ( 0.000037 0.000045 0.000047 ) 0.048447 0.057038 0.133642 ( 0.000029 0.000036 0.000038 ) M - matrix: 0.013847 0.004582 0.009273 ( 0.000010 0.000007 0.000007 ) 0.004582 0.013945 0.009352 ( 0.000007 0.000011 0.000007 ) 0.009273 0.009352 0.018700 ( 0.000007 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.376(4) 7.368(4) 7.350(3) 120.29(5) 120.04(5) 89.65(4) V = 281.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* UB - matrix: 0.117829 0.039162 0.078870 ( 0.000032 0.000039 0.000040 ) 0.000018 0.111472 0.056247 ( 0.000035 0.000042 0.000044 ) -0.000038 -0.000026 0.096439 ( 0.000027 0.000033 0.000034 ) M - matrix: 0.013884 0.004616 0.009291 ( 0.000007 0.000006 0.000006 ) 0.004616 0.013960 0.009356 ( 0.000006 0.000010 0.000007 ) 0.009291 0.009356 0.018685 ( 0.000006 0.000007 0.000010 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 7.369(2) 7.365(3) 7.352(3) 120.23(4) 120.02(4) 89.78(3) V = 281.64(18) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.32 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.087804 -0.044309 0.013053 ( 0.000031 0.000030 0.000036 ) 0.061850 0.094149 0.026136 ( 0.000022 0.000021 0.000025 ) 0.048852 0.055798 0.133161 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013922 0.004658 0.009268 ( 0.000007 0.000004 0.000005 ) 0.004658 0.013941 0.009312 ( 0.000004 0.000005 0.000005 ) 0.009268 0.009312 0.018585 ( 0.000005 0.000005 0.000008 ) unit cell: 7.355(2) 7.365(2) 7.3551(19) 120.06(3) 119.86(3) 90.09(2) V = 281.85(14) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) HKL list info: 1269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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: 0.087791 -0.044307 0.013055 ( 0.000032 0.000030 0.000036 ) 0.061852 0.094148 0.026141 ( 0.000022 0.000021 0.000025 ) 0.048851 0.055805 0.133150 ( 0.000025 0.000024 0.000029 ) M - matrix: 0.013919 0.004660 0.009267 ( 0.000007 0.000004 0.000005 ) 0.004660 0.013941 0.009313 ( 0.000004 0.000005 0.000005 ) 0.009267 0.009313 0.018583 ( 0.000005 0.000005 0.000008 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 7.356(2) 7.366(2) 7.3563(19) 120.07(3) 119.86(3) 90.09(2) V = 281.92(14) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.32 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) UB - matrix: 0.087903 -0.044369 0.012678 ( 0.000021 0.000024 0.000026 ) 0.061483 0.094414 0.026172 ( 0.000019 0.000022 0.000023 ) 0.049390 0.055433 0.133214 ( 0.000017 0.000020 0.000021 ) M - matrix: 0.013947 0.004643 0.009303 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013955 0.009293 ( 0.000004 0.000005 0.000004 ) 0.009303 0.009293 0.018592 ( 0.000004 0.000004 0.000006 ) unit cell: 7.3585(17) 7.3510(18) 7.3581(15) 119.98(2) 120.05(2) 89.95(2) V = 281.39(11) OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 OTKP changes: 223 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) HKL list info: 1296 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087903 -0.044369 0.012678 ( 0.000021 0.000024 0.000026 ) 0.061483 0.094414 0.026172 ( 0.000019 0.000022 0.000023 ) 0.049390 0.055433 0.133214 ( 0.000017 0.000020 0.000021 ) M - matrix: 0.013947 0.004643 0.009303 ( 0.000005 0.000004 0.000004 ) 0.004643 0.013955 0.009293 ( 0.000004 0.000005 0.000004 ) 0.009303 0.009293 0.018592 ( 0.000004 0.000004 0.000006 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3585(17) 7.3510(18) 7.3581(15) 119.98(2) 120.05(2) 89.95(2) V = 281.39(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* UB - matrix: 0.118100 0.039327 0.078777 ( 0.000021 0.000024 0.000026 ) 0.000003 0.111393 0.055619 ( 0.000011 0.000012 0.000013 ) -0.000002 0.000003 0.096401 ( 0.000023 0.000027 0.000029 ) M - matrix: 0.013948 0.004645 0.009304 ( 0.000005 0.000003 0.000004 ) 0.004645 0.013955 0.009294 ( 0.000003 0.000003 0.000004 ) 0.009304 0.009294 0.018592 ( 0.000004 0.000004 0.000007 ) UB fit with 223 obs out of 223 (total:223,skipped:0) (100.00%) unit cell: 7.3582(16) 7.3514(13) 7.358(3) 119.98(3) 120.05(3) 89.965(17) V = 281.39(12) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.32 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) UB - matrix: 0.087891 -0.044458 0.012534 ( 0.000023 0.000026 0.000025 ) 0.061558 0.094486 0.026291 ( 0.000030 0.000034 0.000033 ) 0.049399 0.055218 0.133226 ( 0.000022 0.000025 0.000024 ) M - matrix: 0.013955 0.004637 0.009301 ( 0.000006 0.000005 0.000004 ) 0.004637 0.013953 0.009283 ( 0.000005 0.000007 0.000005 ) 0.009301 0.009283 0.018597 ( 0.000004 0.000005 0.000007 ) unit cell: 7.354(2) 7.348(2) 7.3519(19) 119.95(3) 120.04(3) 89.96(2) V = 281.04(14) OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 Run 5 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) HKL list info: 982 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.087891 -0.044458 0.012534 ( 0.000023 0.000026 0.000025 ) 0.061558 0.094486 0.026291 ( 0.000030 0.000034 0.000033 ) 0.049399 0.055218 0.133226 ( 0.000022 0.000025 0.000024 ) M - matrix: 0.013955 0.004637 0.009301 ( 0.000006 0.000005 0.000004 ) 0.004637 0.013953 0.009283 ( 0.000005 0.000007 0.000005 ) 0.009301 0.009283 0.018597 ( 0.000004 0.000005 0.000007 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 7.354(2) 7.348(2) 7.3519(19) 119.95(3) 120.04(3) 89.96(2) V = 281.04(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 192 obs out of 192 (total:192,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: 0.087891 -0.044458 0.012534 ( 0.000023 0.000026 0.000025 ) 0.061558 0.094486 0.026291 ( 0.000030 0.000034 0.000033 ) 0.049399 0.055218 0.133226 ( 0.000022 0.000025 0.000024 ) M - matrix: 0.013955 0.004637 0.009301 ( 0.000006 0.000005 0.000004 ) 0.004637 0.013953 0.009283 ( 0.000005 0.000007 0.000005 ) 0.009301 0.009283 0.018597 ( 0.000004 0.000005 0.000007 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 7.354(2) 7.348(2) 7.3519(19) 119.95(3) 120.04(3) 89.96(2) V = 281.04(14) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.32 ka= 69.89 ph= 92.09 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\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" PROFFIT INFO: Final refinement of B matrix and unit cell UB - matrix: 0.117703 0.038564 0.078693 ( 0.000037 0.000038 0.000042 ) 0.000010 0.111548 0.056303 ( 0.000029 0.000030 0.000034 ) -0.000043 -0.000097 0.096201 ( 0.000023 0.000024 0.000026 ) M - matrix: 0.013854 0.004540 0.009259 ( 0.000009 0.000006 0.000006 ) 0.004540 0.013930 0.009306 ( 0.000006 0.000007 0.000006 ) 0.009259 0.009306 0.018617 ( 0.000006 0.000006 0.000009 ) UB fit with 1111 obs out of 1120 (total:1120,skipped:0) (99.20%) unit cell: 7.376(2) 7.364(2) 7.368(2) 120.29(3) 120.17(4) 89.46(3) V = 282.33(15) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 101 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof 4870 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:09:20 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.165) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) Run 5 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-571.0000 max=7905880.0000 PROFFIT INFO: signal sum lp corr: min=-635.2561 max=1276360.0893 PROFFIT INFO: background sum: min=-77.0000 max=7581.0000 PROFFIT INFO: background sum sig2: min=405.0000 max=5642.0000 PROFFIT INFO: num of signal pixels: min=38 max=504 PROFFIT INFO: Inet: min=-1016.4097 max=2042176.2500 PROFFIT INFO: sig(Inet): min=52.5702 max=26773.3828 PROFFIT INFO: Inet/sig(Inet): min=-1.71 max=198.32 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 404 1648 2489 3011 3235 3771 4095 4296 4613 4816 4870 Percent 8.3 33.8 51.1 61.8 66.4 77.4 84.1 88.2 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4870 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 4870 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2042176- 132813 487 418935.97 77.26 100.00 132744- 4130 487 30853.49 19.99 100.00 4127- 2141 487 2942.77 7.38 98.77 2138- 1249 487 1630.12 3.92 53.59 1246- 835 487 1021.55 2.34 14.37 835- 563 487 691.62 1.73 7.60 563- 344 487 448.42 1.29 6.16 343- 161 487 249.43 0.72 1.23 160- 21 487 87.62 0.31 0.00 21- -1016 487 -124.51 -0.24 0.00 ------------------------------------------------------------------------------------ 2042176- -1016 4870 45673.65 11.47 38.17 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 487 107055.78 16.79 70.02 1.75- 1.28 487 107913.97 23.13 59.96 1.28- 1.08 487 47496.31 13.28 47.23 1.08- 0.94 487 38865.81 12.33 43.94 0.94- 0.85 487 41675.81 12.36 35.73 0.85- 0.77 487 29909.49 9.65 35.32 0.77- 0.70 487 31395.24 9.65 31.42 0.70- 0.64 487 21398.66 6.91 22.59 0.64- 0.57 487 12326.34 4.49 17.04 0.57- 0.44 487 18699.08 6.11 18.48 ------------------------------------------------------------------------------------ 6.55- 0.44 4870 45673.65 11.47 38.17 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:09:20 2019 Sorting 4870 observations 87 unique observations with > 7.00 F2/sig(F2) 4870 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 103 411 5 0 74 486 Total number of frames 486 Maximum number of 87 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 4870 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 17 36 3 0 16 53 4 0 17 71 5 0 12 84 Total number of frames 84 1189 observations > 7.00 F2/sig(F2) 1189 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 16 35 3 0 16 52 4 0 17 70 5 0 12 83 Total number of frames 83 Removing 'redundancy=1' reflections Average redundancy: 8.6 (Out of 1189 removed 34 = 1155, unique = 134) 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 1155 observations in 5 runs Run # start # end # total # 1 0 17 18 2 0 16 35 3 0 16 52 4 0 17 70 5 0 12 83 Total number of frames 83 134 unique data precomputed (should be 134) 134 unique data with 1155 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.6 (Out of 1155 removed 0 = 1155, unique = 134) 134 unique data precomputed (should be 134) 134 unique data with 1155 observations RMS deviation of equivalent data = 0.39470 Rint = 0.36273 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.35990, wR= 0.47917 Trying model 1 (ne=2, no=0)... Results: Rint= 0.27398, wR= 0.35451, Acormin=0.506, Acormax=1.450, Acor_av=0.983 F test: Probability=1.000, F= 1.717 Trying model 2 (ne=2, no=1)... Results: Rint= 0.25821, wR= 0.34294, Acormin=0.519, Acormax=1.485, Acor_av=0.969 F test: Probability=0.967, F= 1.123 Trying model 3 (ne=4, no=0)... Results: Rint= 0.26762, wR= 0.34866, Acormin=0.516, Acormax=1.478, Acor_av=0.961 F test: Probability=0.000, F= 0.925 Trying model 4 (ne=4, no=1)... Results: Rint= 0.24838, wR= 0.33348, Acormin=0.429, Acormax=1.621, Acor_av=0.958 F test: Probability=0.862, F= 1.071 Trying model 5 (ne=4, no=3)... Results: Rint= 0.23173, wR= 0.30840, Acormin=0.300, Acormax=1.744, Acor_av=0.920 F test: Probability=0.999, F= 1.222 Trying model 6 (ne=6, no=0)... Results: Rint= 0.26414, wR= 0.33541, Acormin=0.324, Acormax=1.594, Acor_av=0.929 F test: Probability=0.000, F= 0.767 Trying model 7 (ne=6, no=1)... Results: Rint= 0.24419, wR= 0.31570, Acormin=0.305, Acormax=1.677, Acor_av=0.949 F test: Probability=0.000, F= 0.895 Trying model 8 (ne=6, no=3)... Results: Rint= 0.23075, wR= 0.29930, Acormin=0.183, Acormax=1.877, Acor_av=0.903 F test: Probability=0.000, F= 0.995 Trying model 9 (ne=6, no=5)... Results: Rint= 0.23180, wR= 0.29721, Acormin=0.295, Acormax=1.905, Acor_av=0.835 F test: Probability=0.000, F= 0.975 Trying model 10 (ne=8, no=0)... Results: Rint= 0.27618, wR= 0.33358, Acormin=0.077, Acormax=1.633, Acor_av=0.845 F test: Probability=0.000, F= 0.690 Trying model 11 (ne=8, no=1)... Results: Rint= 0.31561, wR= 0.36849, Acormin=0.063, Acormax=1.268, Acor_av=0.648 F test: Probability=0.000, F= 0.527 Trying model 12 (ne=8, no=3)... Results: Rint= 0.32623, wR= 0.37466, Acormin=-0.007, Acormax=0.111, Acor_av=0.039 F test: Probability=0.000, F= 0.489 Trying model 13 (ne=8, no=5)... Results: Rint= 0.31148, wR= 0.35936, Acormin=-0.006, Acormax=0.121, Acor_av=0.040 F test: Probability=0.000, F= 0.531 Trying model 14 (ne=8, no=7)... Results: Rint= 0.26084, wR= 0.31679, Acormin=-0.001, Acormax=0.174, Acor_av=0.041 F test: Probability=0.000, F= 0.745 Final absorption model (ne=4, no=3): Rint= 0.23173, Acormin=0.300, Acormax=1.744, Acor_av=0.920 Combined refinement in use Rint: 0.37647 There are 83 active scales (one needs to be fixed) Refinement control: frame scale #80 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 106 pars with 5671 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.39470 Using Levenberg-Marquardt: 0.00010 New wR= 0.22077 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.36273 with corrections 0.18480 Rint for all data: 0.37647 with corrections 0.20063 1 observations identified as outliers and rejected Cycle 2 wR= 0.21991 Using Levenberg-Marquardt: 0.00001 New wR= 0.21533 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.36270 with corrections 0.18068 Rint for all data: 0.37647 with corrections 0.19646 1 observations identified as outliers and rejected Cycle 3 wR= 0.21283 Using Levenberg-Marquardt: 0.00000 New wR= 0.21336 Using Levenberg-Marquardt: 0.00001 New wR= 0.21336 Using Levenberg-Marquardt: 0.00010 New wR= 0.21333 Using Levenberg-Marquardt: 0.00100 New wR= 0.21308 Using Levenberg-Marquardt: 0.01000 New wR= 0.21181 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.36180 with corrections 0.17466 Rint for all data: 0.37647 with corrections 0.19258 0 observations identified as outliers and rejected Cycle 4 wR= 0.21181 Using Levenberg-Marquardt: 0.00100 New wR= 0.21056 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.36180 with corrections 0.17391 Rint for all data: 0.37647 with corrections 0.19161 0 observations identified as outliers and rejected Cycle 5 wR= 0.21056 Using Levenberg-Marquardt: 0.00010 New wR= 0.21129 Using Levenberg-Marquardt: 0.00100 New wR= 0.21119 Using Levenberg-Marquardt: 0.01000 New wR= 0.21070 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.36180 with corrections 0.17359 Rint for all data: 0.37647 with corrections 0.19130 Final wR= 0.21070 Final frame scales: Min= 0.8092 Max= 2.6013 Final absorption correction factors: Amin= 0.0961 Amax= 1.7693 PROFFIT INFO: Inet (after scale3 abspack): min=-3174.0718 max=1351923.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=27.5555 max=27747.2695 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/104 4870 reflections read from tmp file 1254 reflections are rejected (1201 as outliers, 53 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 73 43 38 30 35 18 17 18 158 Initial Chi^2= 2.03704 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.94888 Current error model SIG(F2)^2 = 440.43*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 417.92*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 417.92*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1351924- 127711 487 365441.04 32.45 100.00 127368- 3784 487 27116.26 6.93 83.57 3783- 1969 487 2651.14 2.67 28.34 1969- 1188 487 1544.97 2.07 19.10 1187- 757 487 949.74 1.39 2.26 756- 499 487 620.30 1.16 1.03 498- 306 487 401.69 1.03 0.62 306- 144 487 224.16 0.89 0.62 144- 21 487 77.16 0.52 0.00 21- -3174 487 -151.84 -0.29 0.00 ------------------------------------------------------------------------------------ 1351924- -3174 4870 39887.46 4.88 23.55 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 487 91274.20 11.15 54.83 1.75- 1.28 487 96627.77 9.93 40.66 1.28- 1.08 487 42571.82 5.28 28.95 1.08- 0.94 487 38776.83 4.41 21.77 0.94- 0.85 487 35834.93 4.36 19.30 0.85- 0.77 487 28034.69 3.51 16.63 0.77- 0.70 487 25846.47 3.46 17.45 0.70- 0.64 487 16841.33 2.58 11.91 0.64- 0.57 487 9695.66 1.84 9.65 0.57- 0.44 487 13370.89 2.28 14.37 ------------------------------------------------------------------------------------ 6.55- 0.44 4870 39887.46 4.88 23.55 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.55- 1.75 487 91274.20 11.15 54.83 6.55- 1.28 974 93950.99 10.54 47.74 6.55- 1.08 1461 76824.60 8.79 41.48 6.55- 0.94 1948 67312.66 7.69 36.55 6.55- 0.85 2435 61017.11 7.03 33.10 6.55- 0.77 2922 55520.04 6.44 30.36 6.55- 0.70 3409 51280.96 6.02 28.51 6.55- 0.64 3896 46976.01 5.59 26.44 6.55- 0.57 4383 42833.75 5.17 24.57 6.55- 0.44 4870 39887.46 4.88 23.55 ------------------------------------------------------------------------------------ 6.55- 0.44 4870 39887.46 4.88 23.55 Scale applied to data: s=0.739686 (maximum obs:1351923.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.191; Rsigma 0.051: data 4870 -> merged 486 With outlier rejection... Rint 0.188; Rsigma 0.050: data 4829 -> merged 486 Rejected total: 41, method kkm 33, method Blessing 8 Completeness direct cell (a, b, c) = (6.560, 6.560, 6.560), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.445337, 6.560225 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 7.35 - 1.59 22 22 26.77 100.00 589 1.55 - 1.22 22 22 25.32 100.00 557 1.20 - 1.02 22 22 23.23 100.00 511 1.02 - 0.92 22 22 18.68 100.00 411 0.92 - 0.84 22 22 18.32 100.00 403 0.84 - 0.79 22 22 13.91 100.00 306 0.79 - 0.75 22 22 13.36 100.00 294 0.75 - 0.71 22 22 10.95 100.00 241 0.71 - 0.69 22 22 10.55 100.00 232 0.68 - 0.65 27 29 9.63 93.10 260 --------------------------------------------------------------- 7.35 - 0.65 225 227 16.91 99.12 3804 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:09:20 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.375557 7.363906 7.367731 120.2860 120.1718 89.4564 4829 Reflections read from file xs2212a.hkl 4829 Reflections used for space-group determination (up to diffraction limit of 0.59A); mean (I/sigma) = 4.89 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2407 2407 2420 2403 3617 3210 3219 4829 N (int>3sigma) = 0 279 303 410 280 496 772 776 1136 Mean intensity = 0.0 0.9 0.9 1.3 0.9 1.0 28.5 30.4 29.5 Mean int/sigma = 0.0 1.5 1.5 2.0 1.4 1.6 4.8 5.1 4.9 Lattice type: P chosen Volume: 282.33 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.334 7.352 7.364 119.73 119.83 90.13 Niggli form: a.a = 53.787 b.b = 54.059 c.c = 54.227 b.c = -26.847 a.c = -26.865 a.b = -0.125 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.467 CUBIC F-lattice R(int) = 0.251 [ 4590] Vol = 1129.3 Cell: 10.472 10.397 10.373 89.86 90.09 90.16 Volume: 1129.32 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.519 TETRAGONAL I-lattice R(int) = 0.226 [ 4202] Vol = 564.7 Cell: 7.389 7.368 10.373 90.04 89.83 89.59 Volume: 564.66 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.305 TETRAGONAL I-lattice R(int) = 0.226 [ 4197] Vol = 564.7 Cell: 7.334 7.352 10.472 89.82 90.05 90.13 Volume: 564.66 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.498 TETRAGONAL I-lattice R(int) = 0.226 [ 4202] Vol = 564.7 Cell: 7.368 7.389 10.373 90.17 90.04 90.41 Volume: 564.66 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.311 ORTHORHOMBIC F-lattice R(int) = 0.191 [ 4146] Vol = 1129.3 Cell: 10.373 10.397 10.472 90.16 90.09 89.86 Volume: 1129.32 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.605 ORTHORHOMBIC I-lattice R(int) = 0.194 [ 4124] Vol = 564.7 Cell: 10.373 7.368 7.389 89.59 89.83 90.04 Volume: 564.66 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.224 ORTHORHOMBIC I-lattice R(int) = 0.224 [ 4134] Vol = 564.7 Cell: 7.334 7.352 10.472 90.18 89.95 90.13 Volume: 564.66 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.281 MONOCLINIC I-lattice R(int) = 0.131 [ 3605] Vol = 564.7 Cell: 7.368 10.373 7.389 90.17 90.41 90.04 Volume: 564.66 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.294 MONOCLINIC I-lattice R(int) = 0.188 [ 3603] Vol = 564.7 Cell: 7.364 10.397 7.376 89.78 90.54 90.01 Volume: 564.66 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.281 MONOCLINIC I-lattice R(int) = 0.131 [ 3605] Vol = 564.7 Cell: 7.368 10.373 7.389 90.17 90.41 90.04 Volume: 564.66 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.128 MONOCLINIC I-lattice R(int) = 0.184 [ 3588] Vol = 564.7 Cell: 7.352 7.334 10.472 90.05 90.18 89.87 Volume: 564.66 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.125 MONOCLINIC I-lattice R(int) = 0.189 [ 3611] Vol = 564.7 Cell: 7.334 10.472 7.352 89.82 90.13 90.05 Volume: 564.66 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.209 MONOCLINIC I-lattice R(int) = 0.189 [ 3611] Vol = 564.7 Cell: 7.334 10.472 7.352 90.18 90.13 89.95 Volume: 564.66 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.118 [ 2583] Vol = 282.3 Cell: 7.334 7.352 7.364 119.73 119.83 90.13 Volume: 282.33 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 2420 0 3207 3210 4829 N (int>3sigma) = 0 0 0 0 410 0 779 783 1136 Mean intensity = 0.0 0.0 0.0 0.0 1.3 0.0 29.5 30.3 29.5 Mean int/sigma = 0.0 0.0 0.0 0.0 2.0 0.0 4.9 5.1 4.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.726 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 27 27 350 942 N I>3s 0 0 0 237 0.0 0.0 -0.0 1.7 0.6 0.6 0.1 2.5 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 0.251 4268 Fd-3m 1 1 227 C N N N N 37 2284 0.250 4333 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.471702 10.396962 10.372819 89.8553 90.0906 90.1630 ZERR 1.00 0.000992 0.010533 0.005818 0.0023 0.0021 0.0890 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 849994- 90336 545 541 48 11.3 337779.15 30.43 0.172 0.201 88712- 2275 654 642 48 13.4 9919.64 4.14 0.334 0.157 2249- 1423 910 905 48 18.9 1832.30 2.01 0.846 0.969 1409- 937 725 721 48 15.0 1114.56 1.37 0.746 0.895 935- 717 512 510 48 10.6 821.84 1.17 0.731 0.760 712- 554 438 432 48 9.0 607.09 0.90 0.680 0.743 553- 433 353 350 48 7.3 473.49 0.84 0.673 0.793 431- 302 309 306 48 6.4 376.05 0.74 0.681 0.767 290- 117 245 243 48 5.1 209.95 0.54 0.829 1.110 117- -425 179 179 54 3.3 34.04 0.15 0.966 3.062 ------------------------------------------------------------------------------------------- 849994- -425 4870 4829 486 9.9 39881.56 4.89 0.188 0.209 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-1.14 1257 1249 48 26.0 78380.71 9.02 0.198 0.242 0.027 1.14-0.89 985 979 49 20.0 39757.81 4.71 0.179 0.192 0.056 0.89-0.76 746 739 49 15.1 33647.26 3.99 0.173 0.208 0.072 0.76-0.69 560 555 50 11.1 23786.54 3.28 0.178 0.214 0.080 0.69-0.63 423 422 48 8.8 18171.64 2.70 0.192 0.187 0.098 0.63-0.59 314 309 48 6.4 11537.60 2.07 0.231 0.260 0.121 0.59-0.55 234 230 49 4.7 15962.96 2.54 0.178 0.162 0.109 0.55-0.52 147 146 48 3.0 6099.28 1.45 0.111 0.112 0.163 0.52-0.49 123 120 48 2.5 12847.30 2.27 0.087 0.092 0.117 0.49-0.45 81 80 49 1.6 4545.03 1.12 0.443 0.521 0.198 ------------------------------------------------------------------------------------------------------ inf-0.45 4870 4829 486 9.9 39881.56 4.89 0.188 0.209 0.050 inf-0.65 3831 3804 225 16.9 46801.21 5.57 0.189 0.222 0.045 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-1.14 1249 48 48 100.0 26.0 78380.71 39.91 0.198 0.006 1.14-0.89 979 49 49 100.0 20.0 39757.81 16.80 0.179 0.017 0.89-0.76 739 49 49 100.0 15.1 33647.26 13.62 0.173 0.023 0.76-0.69 555 50 50 100.0 11.1 23786.54 10.22 0.178 0.027 0.69-0.63 422 50 48 96.0 8.8 18171.64 7.69 0.192 0.044 0.63-0.59 309 53 48 90.6 6.4 11537.60 5.00 0.231 0.052 0.59-0.55 230 57 49 86.0 4.7 15962.96 5.79 0.178 0.053 0.55-0.52 146 63 48 76.2 3.0 6099.28 2.57 0.111 0.089 0.52-0.49 120 80 48 60.0 2.5 12847.30 3.58 0.087 0.075 0.49-0.45 80 149 49 32.9 1.6 4545.03 1.41 0.443 0.910 -------------------------------------------------------------------------------------------- inf-0.45 4829 650 486 74.8 9.9 39881.56 18.44 0.188 0.025 inf-0.65 3804 227 225 99.1 16.9 46801.21 21.98 0.189 0.015 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 RRPPROF to HKL transformation matrix: 1.0 1.0 0.0 -1.0 -1.0 -2.0 -1.0 1.0 0.0 No constraint UB - matrix: 0.013221 -0.008893 -0.066344 ( 0.000010 0.000009 0.000009 ) 0.065190 -0.012975 0.014765 ( 0.000010 0.000010 0.000010 ) -0.014478 -0.066321 0.006092 ( 0.000012 0.000011 0.000011 ) M - matrix: 0.004634 -0.000003 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004646 -0.000006 ( 0.000001 0.000001 0.000001 ) -0.000003 -0.000006 0.004657 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.013221 -0.008893 -0.066344 ( 0.000010 0.000009 0.000009 ) 0.065190 -0.012975 0.014765 ( 0.000010 0.000010 0.000010 ) -0.014478 -0.066321 0.006092 ( 0.000012 0.000011 0.000011 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4194(16) 10.4062(16) 10.3943(15) 89.931(12) 89.966(12) 89.961(12) V = 1127.0(3) unit cell: 10.4067(5) 10.4067(5) 10.4067(5) 90.0 90.0 90.0 V = 1127.02(9) 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.165) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.000) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.000) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.000) Run 5 Omega scan: (-6.000 - 69.000,75 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=-571.0000 max=7905880.0000 PROFFIT INFO: signal sum lp corr: min=-635.2561 max=1276360.0893 PROFFIT INFO: background sum: min=-77.0000 max=7581.0000 PROFFIT INFO: background sum sig2: min=405.0000 max=5642.0000 PROFFIT INFO: num of signal pixels: min=38 max=504 PROFFIT INFO: Inet: min=-1016.4097 max=2042176.2500 PROFFIT INFO: sig(Inet): min=52.5702 max=26773.3828 PROFFIT INFO: Inet/sig(Inet): min=-1.71 max=198.32 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 808 3296 4978 6022 6470 7542 8190 8592 9226 9632 9740 Percent 8.3 33.8 51.1 61.8 66.4 77.4 84.1 88.2 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4870 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 4870 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2042176- 132813 487 418935.97 77.26 100.00 132744- 4130 487 30853.49 19.99 100.00 4127- 2141 487 2942.77 7.38 98.77 2138- 1249 487 1630.12 3.92 53.59 1246- 835 487 1021.55 2.34 14.37 835- 563 487 691.62 1.73 7.60 563- 344 487 448.42 1.29 6.16 343- 161 487 249.43 0.72 1.23 160- 21 487 87.62 0.31 0.00 21- -1016 487 -124.51 -0.24 0.00 ------------------------------------------------------------------------------------ 2042176- -1016 4870 45673.65 11.47 38.17 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 487 117444.46 15.42 68.38 1.73- 1.26 487 86738.45 21.41 61.19 1.26- 1.09 487 58849.05 18.34 66.12 1.09- 0.96 487 56281.30 15.33 36.96 0.96- 0.88 487 12213.91 5.71 40.86 0.88- 0.81 487 56816.14 15.92 39.43 0.81- 0.76 487 18561.65 5.72 16.84 0.76- 0.71 487 21131.63 6.90 17.25 0.71- 0.67 487 24910.51 8.11 28.34 0.67- 0.63 487 3789.36 1.85 6.37 ------------------------------------------------------------------------------------ 6.00- 0.63 4870 45673.65 11.47 38.17 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:09:21 2019 Sorting 4870 observations 43 unique observations with > 7.00 F2/sig(F2) 4870 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 1 101 307 4 0 103 411 5 0 74 486 Total number of frames 486 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 12 frame = 1 scale 4870 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 6 43 Total number of frames 43 1189 observations > 7.00 F2/sig(F2) 1189 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 6 43 Total number of frames 43 Removing 'redundancy=1' reflections Average redundancy: 21.9 (Out of 1189 removed 4 = 1185, unique = 54) 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 1185 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 6 43 Total number of frames 43 54 unique data precomputed (should be 54) 54 unique data with 1185 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 21.9 (Out of 1185 removed 0 = 1185, unique = 54) 54 unique data precomputed (should be 54) 54 unique data with 1185 observations RMS deviation of equivalent data = 0.27342 Rint = 0.21841 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.21365, wR= 0.28634 Trying model 1 (ne=2, no=0)... Results: Rint= 0.10803, wR= 0.15254, Acormin=0.548, Acormax=1.423, Acor_av=0.999 F test: Probability=1.000, F= 3.894 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09696, wR= 0.13964, Acormin=0.487, Acormax=1.472, Acor_av=0.969 F test: Probability=1.000, F= 1.238 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09409, wR= 0.14215, Acormin=0.592, Acormax=1.493, Acor_av=0.999 F test: Probability=0.820, F= 1.056 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08379, wR= 0.12600, Acormin=0.489, Acormax=1.605, Acor_av=0.974 F test: Probability=1.000, F= 1.328 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07832, wR= 0.11848, Acormin=0.526, Acormax=1.711, Acor_av=0.993 F test: Probability=0.984, F= 1.137 Final absorption model (ne=4, no=3): Rint= 0.07832, Acormin=0.526, Acormax=1.711, Acor_av=0.993 Combined refinement in use Rint: 0.22025 There are 43 active scales (one needs to be fixed) Refinement control: frame scale #41 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 66 pars with 2211 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.27342 Using Levenberg-Marquardt: 0.00010 New wR= 0.10845 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21841 with corrections 0.07506 Rint for all data: 0.22025 with corrections 0.07782 2 observations identified as outliers and rejected Cycle 2 wR= 0.09995 Using Levenberg-Marquardt: 0.00001 New wR= 0.09402 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21721 with corrections 0.06393 Rint for all data: 0.22025 with corrections 0.06811 1 observations identified as outliers and rejected Cycle 3 wR= 0.08913 Using Levenberg-Marquardt: 0.00000 New wR= 0.08640 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21644 with corrections 0.05734 Rint for all data: 0.22025 with corrections 0.06224 0 observations identified as outliers and rejected Cycle 4 wR= 0.08640 Using Levenberg-Marquardt: 0.00000 New wR= 0.08583 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21644 with corrections 0.05626 Rint for all data: 0.22025 with corrections 0.06124 0 observations identified as outliers and rejected Cycle 5 wR= 0.08583 Using Levenberg-Marquardt: 0.00000 New wR= 0.08548 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.21644 with corrections 0.05577 Rint for all data: 0.22025 with corrections 0.06079 0 observations identified as outliers and rejected Final wR= 0.08548 Final frame scales: Min= 0.8232 Max= 1.0924 Final absorption correction factors: Amin= 0.4879 Amax= 1.4893 PROFFIT INFO: Inet (after scale3 abspack): min=-1014.0037 max=1387594.6250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=37.9039 max=27384.1348 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/104 4870 reflections read from tmp file 234 reflections are rejected (232 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 3 2 4 2 5 3 4 136 Initial Chi^2= 0.51081 Cycle 1, Chi^2= 1.02787 Current error model SIG(F2)^2 = 68.22*I_RAW + 9.03*I_BACK+(0.02970*)^2 Cycle 2, Chi^2= 1.01910 Current error model SIG(F2)^2 = 81.51*I_RAW + 6.45*I_BACK+(0.02484*)^2 Cycle 3, Chi^2= 1.00524 Current error model SIG(F2)^2 = 85.38*I_RAW + 5.90*I_BACK+(0.02443*)^2 Cycle 4, Chi^2= 1.00120 Current error model SIG(F2)^2 = 86.31*I_RAW + 5.79*I_BACK+(0.02439*)^2 Cycle 5, Chi^2= 1.00028 Current error model SIG(F2)^2 = 86.52*I_RAW + 5.76*I_BACK+(0.02438*)^2 Final Chi^2= 1.00028 Final error model SIG(F2)^2 = 86.52*I_RAW + 5.76*I_BACK+(0.02438*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1387595- 123145 487 394940.90 32.49 100.00 123002- 3601 487 30691.37 13.44 100.00 3575- 2095 487 2775.78 6.21 99.79 2093- 1200 487 1585.89 4.04 69.40 1200- 794 487 973.67 2.75 23.82 794- 542 487 664.90 2.40 14.78 541- 342 487 435.32 2.03 9.86 342- 162 487 246.78 1.43 3.49 162- 23 487 87.72 0.79 0.41 22- -1014 487 -122.96 -0.52 0.00 ------------------------------------------------------------------------------------ 1387595- -1014 4870 43227.94 6.50 42.16 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 487 110031.15 10.67 72.07 1.73- 1.26 487 82511.48 9.94 64.68 1.26- 1.09 487 57135.29 8.44 69.82 1.09- 0.96 487 52554.67 7.05 39.22 0.96- 0.88 487 11012.11 4.27 48.05 0.88- 0.81 487 54811.96 8.59 45.79 0.81- 0.76 487 17648.87 3.85 19.92 0.76- 0.71 487 19609.05 4.92 20.94 0.71- 0.67 487 23304.03 5.56 33.06 0.67- 0.63 487 3660.77 1.77 8.01 ------------------------------------------------------------------------------------ 6.00- 0.63 4870 43227.94 6.50 42.16 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 487 110031.15 10.67 72.07 6.00- 1.26 974 96271.31 10.31 68.38 6.00- 1.09 1461 83225.97 9.68 68.86 6.00- 0.96 1948 75558.15 9.03 61.45 6.00- 0.88 2435 62648.94 8.07 58.77 6.00- 0.81 2922 61342.78 8.16 56.61 6.00- 0.76 3409 55100.79 7.54 51.36 6.00- 0.71 3896 50664.32 7.22 47.56 6.00- 0.67 4383 47624.29 7.03 45.95 6.00- 0.63 4870 43227.94 6.50 42.16 ------------------------------------------------------------------------------------ 6.00- 0.63 4870 43227.94 6.50 42.16 Scale applied to data: s=0.720671 (maximum obs:1387594.625,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.061; Rsigma 0.036: data 4870 -> merged 162 With outlier rejection... Rint 0.056; Rsigma 0.036: data 4855 -> merged 162 Rejected total: 15, method kkm 7, method Blessing 8 Completeness direct cell (a, b, c) = (10.407, 10.407, 10.407), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626407, 6.008283 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 7.35 - 1.76 14 14 31.86 100.00 446 1.73 - 1.27 14 14 35.57 100.00 498 1.26 - 1.06 14 14 39.64 100.00 555 1.05 - 0.97 14 14 34.21 100.00 479 0.95 - 0.88 14 14 35.93 100.00 503 0.87 - 0.81 14 14 31.86 100.00 446 0.80 - 0.76 14 14 33.21 100.00 465 0.76 - 0.72 14 14 28.00 100.00 392 0.72 - 0.69 14 14 30.50 100.00 427 0.69 - 0.65 19 19 25.68 100.00 488 --------------------------------------------------------------- 7.35 - 0.65 145 145 32.41 100.00 4699 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:09:20 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 7.375557 7.363906 7.367731 120.2860 120.1718 89.4564 4829 Reflections read from file xs2212a.hkl 4829 Reflections used for space-group determination (up to diffraction limit of 0.59A); mean (I/sigma) = 4.89 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2407 2407 2420 2403 3617 3210 3219 4829 N (int>3sigma) = 0 279 303 410 280 496 772 776 1136 Mean intensity = 0.0 0.9 0.9 1.3 0.9 1.0 28.5 30.4 29.5 Mean int/sigma = 0.0 1.5 1.5 2.0 1.4 1.6 4.8 5.1 4.9 Lattice type: P chosen Volume: 282.33 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.334 7.352 7.364 119.73 119.83 90.13 Niggli form: a.a = 53.787 b.b = 54.059 c.c = 54.227 b.c = -26.847 a.c = -26.865 a.b = -0.125 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.467 CUBIC F-lattice R(int) = 0.251 [ 4590] Vol = 1129.3 Cell: 10.472 10.397 10.373 89.86 90.09 90.16 Volume: 1129.32 Matrix: 1.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.519 TETRAGONAL I-lattice R(int) = 0.226 [ 4202] Vol = 564.7 Cell: 7.389 7.368 10.373 90.04 89.83 89.59 Volume: 564.66 Matrix:-1.0000 -1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.305 TETRAGONAL I-lattice R(int) = 0.226 [ 4197] Vol = 564.7 Cell: 7.334 7.352 10.472 89.82 90.05 90.13 Volume: 564.66 Matrix: 0.0000 1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.498 TETRAGONAL I-lattice R(int) = 0.226 [ 4202] Vol = 564.7 Cell: 7.368 7.389 10.373 90.17 90.04 90.41 Volume: 564.66 Matrix: 0.0000 0.0000 1.0000 1.0000 1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.311 ORTHORHOMBIC F-lattice R(int) = 0.191 [ 4146] Vol = 1129.3 Cell: 10.373 10.397 10.472 90.16 90.09 89.86 Volume: 1129.32 Matrix: 1.0000 -1.0000 0.0000 1.0000 1.0000 2.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.605 ORTHORHOMBIC I-lattice R(int) = 0.194 [ 4124] Vol = 564.7 Cell: 10.373 7.368 7.389 89.59 89.83 90.04 Volume: 564.66 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.224 ORTHORHOMBIC I-lattice R(int) = 0.224 [ 4134] Vol = 564.7 Cell: 7.334 7.352 10.472 90.18 89.95 90.13 Volume: 564.66 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.281 MONOCLINIC I-lattice R(int) = 0.131 [ 3605] Vol = 564.7 Cell: 7.368 10.373 7.389 90.17 90.41 90.04 Volume: 564.66 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.294 MONOCLINIC I-lattice R(int) = 0.188 [ 3603] Vol = 564.7 Cell: 7.364 10.397 7.376 89.78 90.54 90.01 Volume: 564.66 Matrix: 0.0000 1.0000 0.0000 -1.0000 -1.0000 -2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.281 MONOCLINIC I-lattice R(int) = 0.131 [ 3605] Vol = 564.7 Cell: 7.368 10.373 7.389 90.17 90.41 90.04 Volume: 564.66 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.128 MONOCLINIC I-lattice R(int) = 0.184 [ 3588] Vol = 564.7 Cell: 7.352 7.334 10.472 90.05 90.18 89.87 Volume: 564.66 Matrix: 1.0000 0.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.125 MONOCLINIC I-lattice R(int) = 0.189 [ 3611] Vol = 564.7 Cell: 7.334 10.472 7.352 89.82 90.13 90.05 Volume: 564.66 Matrix: 0.0000 -1.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.209 MONOCLINIC I-lattice R(int) = 0.189 [ 3611] Vol = 564.7 Cell: 7.334 10.472 7.352 90.18 90.13 89.95 Volume: 564.66 Matrix: 0.0000 1.0000 1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.118 [ 2583] Vol = 282.3 Cell: 7.334 7.352 7.364 119.73 119.83 90.13 Volume: 282.33 Matrix: 0.0000 1.0000 1.0000 -1.0000 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 2420 0 3207 3210 4829 N (int>3sigma) = 0 0 0 0 410 0 779 783 1136 Mean intensity = 0.0 0.0 0.0 0.0 1.3 0.0 29.5 30.3 29.5 Mean int/sigma = 0.0 0.0 0.0 0.0 2.0 0.0 4.9 5.1 4.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 2.726 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 27 27 350 942 N I>3s 0 0 0 237 0.0 0.0 -0.0 1.7 0.6 0.6 0.1 2.5 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 0.251 4268 Fd-3m 1 1 227 C N N N N 37 2284 0.250 4333 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 xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.471702 10.396962 10.372819 89.8553 90.0906 90.1630 ZERR 1.00 0.000992 0.010533 0.005818 0.0023 0.0021 0.0890 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1169220- 95074 595 586 27 21.7 344518.87 30.44 0.052 0.065 80917- 1869 924 920 27 34.1 5428.42 8.41 0.103 0.134 1753- 803 955 954 27 35.3 1171.94 3.04 0.224 0.298 767- 332 1022 1022 27 37.9 507.50 2.00 0.370 0.520 330- 72 654 653 27 24.2 224.08 1.18 0.604 0.977 63- -103 720 720 27 26.7 13.50 0.21 0.960 4.044 ------------------------------------------------------------------------------------------- 1169220- -103 4870 4855 162 30.0 42981.45 6.48 0.056 0.069 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-1.27 945 943 27 34.9 99004.58 10.57 0.048 0.060 0.027 1.26-0.97 1006 1002 27 37.1 52463.06 7.51 0.049 0.061 0.032 0.97-0.81 908 905 27 33.5 35100.51 6.76 0.061 0.077 0.041 0.81-0.73 873 872 27 32.3 11077.13 3.10 0.072 0.079 0.062 0.73-0.67 723 721 27 26.7 27226.82 6.06 0.088 0.114 0.055 0.67-0.63 415 412 27 15.3 4101.66 1.88 0.148 0.112 0.124 ------------------------------------------------------------------------------------------------------ inf-0.63 4870 4855 162 30.0 42981.45 6.48 0.056 0.069 0.036 inf-0.65 4710 4698 144 32.6 44171.86 6.62 0.056 0.068 0.035 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-1.27 943 27 27 100.0 34.9 99004.58 59.83 0.048 0.007 1.26-0.97 1002 27 27 100.0 37.1 52463.06 42.86 0.049 0.007 0.97-0.81 905 27 27 100.0 33.5 35100.51 40.09 0.061 0.009 0.81-0.73 872 27 27 100.0 32.3 11077.13 16.69 0.072 0.013 0.73-0.67 721 27 27 100.0 26.7 27226.82 32.47 0.088 0.011 0.67-0.63 412 27 27 100.0 15.3 4101.66 7.83 0.148 0.034 -------------------------------------------------------------------------------------------- inf-0.63 4855 162 162 100.0 30.0 42981.45 36.42 0.056 0.009 inf-0.65 4698 144 144 100.0 32.6 44171.86 37.42 0.056 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC FULLAUTOANALYSECONCURRENT Process information (Wed Aug 21 14:14:48 2019) ID: 3668; threads 40; handles 812; mem 526472.00 (1207128.00)kB; time: 1w 5d 0h 25m 35s MEMORY INFO: Memory PF:245.0, Ph:569.0, V:1176.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:511.9,peak PF: 700.2, WS: 479.5, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#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 Wed Aug 21 14:14:48 2019 AUTO INFO: Experiment: D:\Data\xs2212a\xs2212a.run AUTO INFO: Clearing peak tables (hunting=200000 peaks,xyz=100000 peaks) MACHINE INFORMATION - GONIOMETER (RIGAKU) OXFORD DIFFRACTION/AGILENT TECHNOLOGIES KM4 XCALIBUR - ALPHA (DEG) 50.02902 BETA (DEG) -0.00070 - WAVELENGTH MO (ANG): A1 0.70930 A2 0.71359 B1 0.63229 - POLARISATION FACTOR 0.50000 - X-RAY BEAM ORIENTATION (DEG): X2 -0.00424 X3 0.00000 - BEAM PATH ABSORPTIONCOEFFICIENTS (MM-1): AIR 0.00013 BE 0.04736 - BE THICKNESS (MM): 0.50000 - SOFTWARE ZEROCORRECTION (DEG): OMEGA -0.00378 THETA -0.13900 KAPPA -0.11263 PHI 0.00000 DETECTOR 0.00000 - MACHINE OFFSETS (STEPS): OMEGA 0 THETA 0 KAPPA 0 PHI 0 DETECTOR 133408 - 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 0.72800 X2 -0.07900 X3 0.00000 - DETECTOR DISTANCE (MM): 53.00000 - DETECTOR ZERO (PIX, 1X1 BINNING): X 1028.43100 Y 1027.41100 - 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 xs2212a\xs2212a.par ******************************************************************************************************* Auto analyse stage: PEAK HUNTING (Wed Aug 21 14:14:48 2019) ******************************************************************************************************* 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= -24.44 ka= -68.11 ph= 119.34 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= -68.11 ph= -24.52 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= -66.11 ph= -128.46 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 68.89 ph= 0.28 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 24.32 ka= 69.89 ph= 92.09 AUTO INFO: 2250 peaks in the peak location table 2250 peak locations are merged to 1258 profiles (Parameters: ofix = 2.00, otan(th) = 0.00) We have put 1258 unindexed peaks to the CrysAlis peak table (1258 with profile info) ******************************************************************************************************* Auto analyse stage: CELL FINDING (Wed Aug 21 14:14:53 2019) ******************************************************************************************************* Instrument model: dd: 53.00, x0: 1028.43, y0: 1027.41, beam: -0.00, o0: -0.00, t0: -0.14, k0: -0.11 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 1566411293! 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: 1 387(sub) 882(all), cF( 1,12) 10.41 10.42 10.39 90.14 89.95 90.05 pr: 281.59, r: 1126.35 UM TTTSOLUTION 2: 2 368(sub) 874(all), oI(42, 4) 7.37 10.40 22.08 90.07 89.97 90.12 pr: 845.41, r: 1690.82 Peak table: 500(sub) 1258(all) Best cell: 387 indexed, Niggli cF( 1,12): 10.41 10.42 10.39 90.14 89.95 90.05 prim: 281.59, red: 1126.35 UM TTTSOLUTION 1: 3 373(sub) 951(all), hP(12, 9) 7.33 7.36 18.00 90.11 89.80 119.63 pr: 844.88, r: 844.88 UM TTTSOLUTION 2: 4 387(sub) 882(all), cF( 1,12) 10.41 10.42 10.39 90.14 89.95 90.05 pr: 281.59, r: 1126.35 UM TTTSOLUTION 3: 5 349(sub) 758(all), tI(15, 7) 10.39 10.43 20.83 89.84 89.75 89.75 pr: 1128.71, r: 2257.42 Peak table: 500(sub) 1258(all) Best cell: 373 indexed, Niggli hP(12, 9): 7.33 7.36 18.00 90.11 89.80 119.63 prim: 844.88, red: 844.88 UM TTTSOLUTION 1: 6 373(sub) 951(all), hP(12, 9) 7.33 7.36 18.00 90.11 89.80 119.63 pr: 844.88, r: 844.88 UM TTTSOLUTION 2: 7 387(sub) 882(all), cF( 1,12) 10.41 10.42 10.39 90.14 89.95 90.05 pr: 281.59, r: 1126.35 UM TTTSOLUTION 3: 8 365(sub) 778(all), hR( 9, 8) 7.35 7.36 36.05 89.88 90.12 119.94 pr: 563.31, r: 1689.93 UM TTTSOLUTION 4: 9 349(sub) 758(all), tI(15, 7) 10.39 10.43 20.83 89.84 89.75 89.75 pr: 1128.71, r: 2257.42 Peak table: 500(sub) 1258(all) Best cell: 373 indexed, Niggli hP(12, 9): 7.33 7.36 18.00 90.11 89.80 119.63 prim: 844.88, red: 844.88 UM TTTSOLUTION 1: 10 373(sub) 951(all), hP(12, 9) 7.33 7.36 18.00 90.11 89.80 119.63 pr: 844.88, r: 844.88 UM TTTSOLUTION 2: 11 387(sub) 882(all), cF( 1,12) 10.41 10.42 10.39 90.14 89.95 90.05 pr: 281.59, r: 1126.35 UM TTTSOLUTION 3: 12 365(sub) 778(all), hR( 9, 8) 7.35 7.36 36.05 89.88 90.12 119.94 pr: 563.31, r: 1689.93 UM TTTSOLUTION 4: 13 349(sub) 758(all), tI(15, 7) 10.39 10.43 20.83 89.84 89.75 89.75 pr: 1128.71, r: 2257.42 Peak table: 500(sub) 1258(all) Best cell: 373 indexed, Niggli hP(12, 9): 7.33 7.36 18.00 90.11 89.80 119.63 prim: 844.88, red: 844.88 UM TTTSOLUTION 1: 14 373(sub) 951(all), hP(12, 9) 7.33 7.36 18.00 90.11 89.80 119.63 pr: 844.88, r: 844.88 UM TTTSOLUTION 2: 15 387(sub) 882(all), cF( 1,12) 10.41 10.42 10.39 90.14 89.95 90.05 pr: 281.59, r: 1126.35 UM TTTSOLUTION 3: 16 349(sub) 758(all), tI(15, 7) 10.39 10.43 20.83 89.84 89.75 89.75 pr: 1128.71, r: 2257.42 Peak table: 500(sub) 1258(all) Best cell: 373 indexed, Niggli hP(12, 9): 7.33 7.36 18.00 90.11 89.80 119.63 prim: 844.88, red: 844.88 Make subset: 0.00017 Make T-vectors: 0.42625 Make unit cell: 0.53925 UM TTT INFO: Volume check Primitive unit cell refinement volume check UB fit with 956 obs out of 1258 (total:1258,skipped:0) (75.99%) UB - matrix: -0.059606 -0.043322 0.014871 ( 0.000037 0.000034 0.000013 ) -0.067148 0.036285 -0.031304 ( 0.000034 0.000031 0.000012 ) 0.065766 -0.095487 -0.018718 ( 0.000044 0.000041 0.000015 ) M - matrix: 0.012387 -0.006134 -0.000015 ( 0.000009 0.000006 0.000002 ) -0.006134 0.012311 0.000007 ( 0.000006 0.000009 0.000002 ) -0.000015 0.000007 0.001551 ( 0.000002 0.000002 0.000001 ) unit cell: 7.343(3) 7.366(3) 18.008(6) 89.99(3) 89.82(3) 60.22(4) V = 845.3(5) UB fit with 966 obs out of 1258 (total:1258,skipped:0) (76.79%) UB - matrix: -0.059572 -0.043265 0.014870 ( 0.000038 0.000035 0.000013 ) -0.067140 0.036295 -0.031282 ( 0.000034 0.000032 0.000012 ) 0.065809 -0.095610 -0.018736 ( 0.000044 0.000041 0.000015 ) M - matrix: 0.012387 -0.006151 -0.000019 ( 0.000009 0.000006 0.000002 ) -0.006151 0.012330 0.000013 ( 0.000006 0.000009 0.000002 ) -0.000019 0.000013 0.001551 ( 0.000002 0.000002 0.000001 ) unit cell: 7.348(3) 7.365(3) 18.012(6) 90.05(3) 89.81(3) 60.15(4) V = 845.4(5) UB fit with 960 obs out of 1258 (total:1258,skipped:0) (76.31%) UB - matrix: -0.059565 -0.043240 0.014865 ( 0.000038 0.000035 0.000013 ) -0.067153 0.036276 -0.031271 ( 0.000034 0.000032 0.000012 ) 0.065844 -0.095644 -0.018742 ( 0.000044 0.000040 0.000015 ) M - matrix: 0.012393 -0.006158 -0.000020 ( 0.000009 0.000006 0.000002 ) -0.006158 0.012333 0.000015 ( 0.000006 0.000009 0.000002 ) -0.000020 0.000015 0.001550 ( 0.000002 0.000002 0.000001 ) unit cell: 7.348(3) 7.366(3) 18.016(6) 90.09(3) 89.82(3) 60.13(4) V = 845.5(5) UM TTT INFO: Smaller volume found! Before: 845.49 after: 281.83 UB fit with 1028 obs out of 1258 (total:1258,skipped:0) (81.72%) UB - matrix: -0.044622 0.029832 -0.058085 ( 0.000043 0.000051 0.000040 ) 0.093786 0.129670 0.067660 ( 0.000047 0.000056 0.000044 ) 0.056246 -0.028277 -0.076910 ( 0.000044 0.000053 0.000041 ) M - matrix: 0.013951 0.009240 0.004612 ( 0.000011 0.000009 0.000007 ) 0.009240 0.018504 0.009215 ( 0.000009 0.000015 0.000009 ) 0.004612 0.009215 0.013867 ( 0.000007 0.000009 0.000010 ) unit cell: 7.341(4) 7.352(4) 7.364(4) 119.89(6) 90.06(4) 119.87(6) V = 281.9(2) UM TTT INFO: Updated best solution UM TTTSOLUTION 1: 14 407(sub) 1025(all), cF( 1,12) 10.39 10.43 10.40 90.11 89.80 90.20 pr: 281.83, r: 1127.32 Primitive unit cell refinement UB fit with 1025 obs out of 1258 (total:1258,skipped:0) (81.48%) UB - matrix: -0.044629 0.029837 -0.058071 ( 0.000043 0.000051 0.000039 ) 0.093800 0.129684 0.067712 ( 0.000048 0.000057 0.000044 ) 0.056243 -0.028258 -0.076911 ( 0.000045 0.000053 0.000041 ) M - matrix: 0.013953 0.009243 0.004617 ( 0.000011 0.000009 0.000007 ) 0.009243 0.018507 0.009222 ( 0.000009 0.000015 0.000009 ) 0.004617 0.009222 0.013872 ( 0.000007 0.000009 0.000010 ) unit cell: 7.341(4) 7.353(4) 7.364(4) 119.90(6) 90.07(4) 119.87(6) V = 281.9(2) No constraint UB - matrix: 0.066226 0.014968 0.006744 ( 0.000019 0.000021 0.000020 ) -0.015883 0.064865 0.013031 ( 0.000016 0.000017 0.000017 ) -0.003843 -0.014203 0.066583 ( 0.000019 0.000021 0.000020 ) M - matrix: 0.004653 0.000016 -0.000016 ( 0.000003 0.000002 0.000002 ) 0.000016 0.004633 0.000001 ( 0.000002 0.000002 0.000002 ) -0.000016 0.000001 0.004649 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.066226 0.014968 0.006744 ( 0.000019 0.000021 0.000020 ) -0.015883 0.064865 0.013031 ( 0.000016 0.000017 0.000017 ) -0.003843 -0.014203 0.066583 ( 0.000019 0.000021 0.000020 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) UB fit with 892 obs out of 1258 (total:1258,skipped:0) (70.91%) unit cell: 10.399(3) 10.421(3) 10.403(3) 90.01(2) 89.80(2) 90.19(2) V = 1127.3(5) unit cell: 10.4074(10) 10.4074(10) 10.4074(10) 90.0 90.0 90.0 V = 1127.28(19) AUTO INFO: Dirax ended... LAMBDA HALF REJECTION: Number of processed reflections: 830 Number of skipped reflections, because of (potential) lambda half effect: 157 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 1566411294! 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: 1 386(sub) 817(all), cF( 1,12) 10.43 10.42 10.37 90.33 90.00 90.09 pr: 281.74, r: 1126.96 UM TTTSOLUTION 2: 2 358(sub) 721(all), hR( 9, 8) 7.36 7.35 36.06 90.00 90.10 119.90 pr: 563.66, r: 1690.97 UM TTTSOLUTION 3: 3 312(sub) 700(all), oC(23, 4) 14.71 20.77 7.37 90.10 89.98 89.99 pr: 1125.84, r: 2251.68 Peak table: 500(sub) 1199(all) Best cell: 386 indexed, Niggli cF( 1,12): 10.43 10.42 10.37 90.33 90.00 90.09 prim: 281.74, red: 1126.96 UM TTTSOLUTION 1: 4 386(sub) 817(all), cF( 1,12) 10.43 10.42 10.37 90.33 90.00 90.09 pr: 281.74, r: 1126.96 UM TTTSOLUTION 2: 5 358(sub) 721(all), hR( 9, 8) 7.36 7.35 36.06 90.00 90.10 119.90 pr: 563.66, r: 1690.97 UM TTTSOLUTION 3: 6 312(sub) 700(all), oC(23, 4) 14.71 20.77 7.37 90.10 89.98 89.99 pr: 1125.84, r: 2251.68 Peak table: 500(sub) 1199(all) Best cell: 386 indexed, Niggli cF( 1,12): 10.43 10.42 10.37 90.33 90.00 90.09 prim: 281.74, red: 1126.96 UM TTTSOLUTION 1: 7 386(sub) 817(all), cF( 1,12) 10.43 10.42 10.37 90.33 90.00 90.09 pr: 281.74, r: 1126.96 UM TTTSOLUTION 2: 8 358(sub) 721(all), hR( 9, 8) 7.36 7.35 36.06 90.00 90.10 119.90 pr: 563.66, r: 1690.97 UM TTTSOLUTION 3: 9 312(sub) 700(all), oC(23, 4) 14.71 20.77 7.37 90.10 89.98 89.99 pr: 1125.84, r: 2251.68 Peak table: 500(sub) 1199(all) Best cell: 386 indexed, Niggli cF( 1,12): 10.43 10.42 10.37 90.33 90.00 90.09 prim: 281.74, red: 1126.96 UM TTTSOLUTION 1: 10 386(sub) 817(all), cF( 1,12) 10.43 10.42 10.37 90.33 90.00 90.09 pr: 281.74, r: 1126.96 UM TTTSOLUTION 2: 11 358(sub) 721(all), hR( 9, 8) 7.36 7.35 36.06 90.00 90.10 119.90 pr: 563.66, r: 1690.97 UM TTTSOLUTION 3: 12 312(sub) 700(all), oC(23, 4) 14.71 20.77 7.37 90.10 89.98 89.99 pr: 1125.84, r: 2251.68 Peak table: 500(sub) 1199(all) Best cell: 386 indexed, Niggli cF( 1,12): 10.43 10.42 10.37 90.33 90.00 90.09 prim: 281.74, red: 1126.96 Make subset: 0.00014 Make T-vectors: 0.36245 Make unit cell: 0.42892 UM TTT INFO: Volume check Primitive unit cell refinement volume check UB fit with 976 obs out of 1199 (total:1258,skipped:59) (81.40%) UB - matrix: 0.029417 0.087827 0.074313 ( 0.000058 0.000049 0.000049 ) 0.129689 0.062013 0.035728 ( 0.000053 0.000044 0.000044 ) -0.028465 0.048483 -0.084399 ( 0.000053 0.000044 0.000044 ) M - matrix: 0.018495 0.009246 0.009222 ( 0.000015 0.000009 0.000009 ) 0.009246 0.013910 0.004650 ( 0.000009 0.000011 0.000008 ) 0.009222 0.004650 0.013922 ( 0.000009 0.000008 0.000011 ) unit cell: 7.351(4) 7.360(4) 7.346(4) 90.25(4) 119.74(5) 119.89(5) V = 282.0(2) UB fit with 994 obs out of 1199 (total:1258,skipped:59) (82.90%) UB - matrix: 0.029644 0.087898 0.074407 ( 0.000057 0.000047 0.000047 ) 0.129694 0.061944 0.035836 ( 0.000052 0.000043 0.000043 ) -0.028313 0.048581 -0.084439 ( 0.000053 0.000044 0.000044 ) M - matrix: 0.018501 0.009264 0.009244 ( 0.000014 0.000009 0.000009 ) 0.009264 0.013923 0.004658 ( 0.000009 0.000011 0.000008 ) 0.009244 0.004658 0.013951 ( 0.000009 0.000008 0.000011 ) unit cell: 7.359(4) 7.361(4) 7.343(4) 90.18(4) 119.80(5) 119.96(5) V = 281.9(2) UB fit with 999 obs out of 1199 (total:1258,skipped:59) (83.32%) UB - matrix: 0.029722 0.087904 0.074435 ( 0.000057 0.000047 0.000048 ) 0.129697 0.061912 0.035909 ( 0.000052 0.000043 0.000044 ) -0.028259 0.048617 -0.084468 ( 0.000053 0.000044 0.000044 ) M - matrix: 0.018503 0.009269 0.009257 ( 0.000014 0.000009 0.000009 ) 0.009269 0.013924 0.004660 ( 0.000009 0.000011 0.000008 ) 0.009257 0.004660 0.013965 ( 0.000009 0.000008 0.000011 ) unit cell: 7.363(4) 7.363(4) 7.342(4) 90.14(4) 119.84(5) 119.98(5) V = 281.9(2) UM TTT INFO: No smaller volume found Primitive unit cell refinement UB fit with 976 obs out of 1199 (total:1258,skipped:59) (81.40%) UB - matrix: 0.029417 0.087827 0.074313 ( 0.000058 0.000049 0.000049 ) 0.129689 0.062013 0.035728 ( 0.000053 0.000044 0.000044 ) -0.028465 0.048483 -0.084399 ( 0.000053 0.000044 0.000044 ) M - matrix: 0.018495 0.009246 0.009222 ( 0.000015 0.000009 0.000009 ) 0.009246 0.013910 0.004650 ( 0.000009 0.000011 0.000008 ) 0.009222 0.004650 0.013922 ( 0.000009 0.000008 0.000011 ) unit cell: 7.351(4) 7.360(4) 7.346(4) 90.25(4) 119.74(5) 119.89(5) V = 282.0(2) No constraint UB - matrix: -0.066351 0.014792 -0.006831 ( 0.000020 0.000021 0.000021 ) 0.015920 0.064901 -0.013071 ( 0.000016 0.000017 0.000017 ) 0.003831 -0.014230 -0.066459 ( 0.000018 0.000018 0.000019 ) M - matrix: 0.004671 -0.000003 -0.000010 ( 0.000003 0.000002 0.000002 ) -0.000003 0.004633 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000010 -0.000004 0.004634 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.066351 0.014792 -0.006831 ( 0.000020 0.000021 0.000021 ) 0.015920 0.064901 -0.013071 ( 0.000016 0.000017 0.000017 ) 0.003831 -0.014230 -0.066459 ( 0.000018 0.000018 0.000019 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000001 ) UB fit with 820 obs out of 1199 (total:1258,skipped:59) (68.39%) unit cell: 10.379(3) 10.420(3) 10.419(3) 89.95(2) 89.88(2) 89.97(2) V = 1126.8(5) unit cell: 10.4061(10) 10.4061(10) 10.4061(10) 90.0 90.0 90.0 V = 1126.84(18) AUTO INFO: Dirax ended... Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" ******************************************************************************************************* Auto analyse stage: MODEL REFINEMENT (Wed Aug 21 14:14:55 2019) ******************************************************************************************************* UB fit with 875 obs out of 1258 (total:1258,skipped:0) (69.55%) UB - matrix: -0.066298 0.014841 -0.006855 ( 0.000019 0.000021 0.000020 ) 0.015886 0.064912 -0.013030 ( 0.000016 0.000018 0.000017 ) 0.003864 -0.014234 -0.066522 ( 0.000019 0.000020 0.000020 ) M - matrix: 0.004663 -0.000008 -0.000010 ( 0.000003 0.000002 0.000002 ) -0.000008 0.004636 -0.000001 ( 0.000002 0.000002 0.000002 ) -0.000010 -0.000001 0.004642 ( 0.000002 0.000002 0.000003 ) unit cell: 10.388(3) 10.417(3) 10.411(3) 89.99(2) 89.88(2) 89.90(2) V = 1126.5(5) OTKP changes: 160 2 4 5 Cycle 1 - Res: 0.042434, da=0.038701, sx=0.003357, sy=0.004341, h=0.010423, k=0.009547, l=0.008544, LM=0.000000 Cycle 2 - Res: 0.034016, da=0.030481, sx=0.003102, sy=0.003834, h=0.008740, k=0.008759, l=0.007110, LM=0.000000 Cycle 3 - Res: 0.034000, da=0.030463, sx=0.003102, sy=0.003835, h=0.008740, k=0.008759, l=0.007110, LM=0.000000 Cycle 4 - Res: 0.034000, da=0.030463, sx=0.003102, sy=0.003835, h=0.008740, k=0.008759, l=0.007110, LM=0.000000 Model change (all parameters): Omega Offset -0.003780 0.085649 0.0894286 6.75646e-006 1 Kappa Offset -0.112630 -0.112630 0 0 0 Phi Offset 0.000000 0.000000 0 0 0 Alpha Value 50.029020 50.029020 0 0 0 Beta Value -0.000700 -0.000700 0 0 0 Theta Offset -0.139000 -0.142281 -0.00328104 9.33907e-006 1 Det. D. Scale 53.000000 53.098497 0.0984968 9.31697e-006 1 Det. Offset X 1028.431000 1028.463598 0.0325976 0.000201798 1 Det. Offset Y 1027.411000 1025.668784 -1.74222 0.000227577 1 Det. Rot. X 0.728000 0.597782 -0.130218 4.57059e-006 1 Det. Rot. Y -0.079000 0.099478 0.178478 9.92644e-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 -0.004240 0.183671 0.187911 5.42722e-006 1 Beam. Rot. Z 0.000000 0.000000 0 0 0 Cryst. Rot. X 167.919490 167.775845 -0.143645 5.56495e-006 1 Cryst. Rot. Y 3.244336 3.036915 -0.20742 5.25663e-006 1 Cryst. Rot. Z -166.525280 -166.315167 0.210114 7.62154e-006 1 Rec. latt. a* 0.096270 0.096113 -0.000156257 1.38442e-008 1 Rec. latt. b* 0.095997 0.095914 -8.34296e-005 1.34744e-008 1 Rec. latt. c* 0.096055 0.095975 -8.02392e-005 1.34614e-008 1 Rec. latt. al* 90.007765 89.954638 -0.0531265 6.89246e-006 1 Rec. latt. be* 90.118079 90.069098 -0.0489808 7.09254e-006 1 Rec. latt. ga* 90.095293 90.039933 -0.05536 6.98669e-006 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: -0.066101 0.015059 -0.006767 ( 0.000016 0.000018 0.000017 ) 0.016067 0.064781 -0.013086 ( 0.000014 0.000016 0.000015 ) 0.003714 -0.014380 -0.066503 ( 0.000016 0.000018 0.000017 ) M - matrix: 0.004641 -0.000008 -0.000010 ( 0.000002 0.000002 0.000002 ) -0.000008 0.004630 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000010 0.000007 0.004640 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.066101 0.015059 -0.006767 ( 0.000016 0.000018 0.000017 ) 0.016067 0.064781 -0.013086 ( 0.000014 0.000016 0.000015 ) 0.003714 -0.014380 -0.066503 ( 0.000016 0.000018 0.000017 ) M - matrix: 0.004637 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004637 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004637 ( 0.000000 0.000000 0.000001 ) UB fit with 929 obs out of 1258 (total:1258,skipped:0) (73.85%) unit cell: 10.411(2) 10.424(2) 10.413(3) 90.08(2) 89.88(2) 89.90(2) V = 1130.1(5) unit cell: 10.4162(9) 10.4162(9) 10.4162(9) 90.0 90.0 90.0 V = 1130.14(17) No constraint UB - matrix: -0.066086 0.015074 -0.006780 ( 0.000016 0.000018 0.000018 ) 0.016042 0.064776 -0.013067 ( 0.000015 0.000016 0.000016 ) 0.003775 -0.014364 -0.066534 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004639 -0.000011 -0.000013 ( 0.000002 0.000002 0.000002 ) -0.000011 0.004629 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000013 0.000007 0.004643 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.066086 0.015074 -0.006780 ( 0.000016 0.000018 0.000018 ) 0.016042 0.064776 -0.013067 ( 0.000015 0.000016 0.000016 ) 0.003775 -0.014364 -0.066534 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004637 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004637 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004637 ( 0.000000 0.000000 0.000001 ) UB fit with 926 obs out of 1258 (total:1258,skipped:0) (73.61%) unit cell: 10.414(2) 10.425(2) 10.409(3) 90.09(2) 89.84(2) 89.86(2) V = 1130.0(5) unit cell: 10.4159(9) 10.4159(9) 10.4159(9) 90.0 90.0 90.0 V = 1130.04(18) No constraint UB - matrix: -0.066074 0.015081 -0.006789 ( 0.000016 0.000018 0.000018 ) 0.016029 0.064770 -0.013062 ( 0.000015 0.000017 0.000016 ) 0.003819 -0.014361 -0.066551 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004637 -0.000013 -0.000015 ( 0.000002 0.000002 0.000002 ) -0.000013 0.004629 0.000007 ( 0.000002 0.000002 0.000002 ) -0.000015 0.000007 0.004646 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.066074 0.015081 -0.006789 ( 0.000016 0.000018 0.000018 ) 0.016029 0.064770 -0.013062 ( 0.000015 0.000017 0.000016 ) 0.003819 -0.014361 -0.066551 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004636 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004636 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004636 ( 0.000000 0.000000 0.000001 ) UB fit with 928 obs out of 1258 (total:1258,skipped:0) (73.77%) unit cell: 10.416(2) 10.426(2) 10.406(3) 90.09(2) 89.82(2) 89.84(2) V = 1130.1(5) unit cell: 10.4160(10) 10.4160(10) 10.4160(10) 90.0 90.0 90.0 V = 1130.05(18) ******************************************************************************************************* Auto analyse stage: CELL FINDING (Wed Aug 21 14:14:56 2019) ******************************************************************************************************* 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 1566411296! 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: 1 409(sub) 928(all), cF( 1,12) 10.40 10.41 10.44 90.13 90.08 90.18 pr: 282.56, r: 1130.22 UM TTTSOLUTION 2: 2 324(sub) 947(all), hP(12, 9) 7.35 7.35 18.08 90.19 89.99 119.80 pr: 847.97, r: 847.97 UM TTTSOLUTION 3: 3 346(sub) 902(all), oP(32, 3) 7.35 10.41 14.78 89.90 89.88 89.85 pr: 1131.39, r: 1131.39 UM TTTSOLUTION 4: 4 336(sub) 777(all), mI(27, 2) 18.07 7.35 22.10 90.07 105.60 90.01 pr: 1414.09, r: 2828.17 UM TTTSOLUTION 5: 5 365(sub) 744(all), hR( 9, 8) 7.37 7.36 36.16 90.00 90.14 120.14 pr: 565.17, r: 1695.50 Peak table: 500(sub) 1258(all) Best cell: 409 indexed, Niggli cF( 1,12): 10.40 10.41 10.44 90.13 90.08 90.18 prim: 282.56, red: 1130.22 UM TTTSOLUTION 1: 6 409(sub) 928(all), cF( 1,12) 10.40 10.41 10.44 90.13 90.08 90.18 pr: 282.56, r: 1130.22 UM TTTSOLUTION 2: 7 324(sub) 947(all), hP(12, 9) 7.35 7.35 18.08 90.19 89.99 119.80 pr: 847.97, r: 847.97 UM TTTSOLUTION 3: 8 346(sub) 902(all), oP(32, 3) 7.35 10.41 14.78 89.90 89.88 89.85 pr: 1131.39, r: 1131.39 UM TTTSOLUTION 4: 9 336(sub) 777(all), mI(27, 2) 18.07 7.35 22.10 90.07 105.60 90.01 pr: 1414.09, r: 2828.17 UM TTTSOLUTION 5: 10 365(sub) 744(all), hR( 9, 8) 7.37 7.36 36.16 90.00 90.14 120.14 pr: 565.17, r: 1695.50 Peak table: 500(sub) 1258(all) Best cell: 409 indexed, Niggli cF( 1,12): 10.40 10.41 10.44 90.13 90.08 90.18 prim: 282.56, red: 1130.22 UM TTTSOLUTION 1: 11 409(sub) 928(all), cF( 1,12) 10.40 10.41 10.44 90.13 90.08 90.18 pr: 282.56, r: 1130.22 UM TTTSOLUTION 2: 12 324(sub) 947(all), hP(12, 9) 7.35 7.35 18.08 90.19 89.99 119.80 pr: 847.97, r: 847.97 UM TTTSOLUTION 3: 13 336(sub) 777(all), mI(27, 2) 18.07 7.35 22.10 90.07 105.60 90.01 pr: 1414.09, r: 2828.17 UM TTTSOLUTION 4: 14 342(sub) 769(all), tI(15, 7) 10.42 10.42 20.76 89.75 89.89 90.31 pr: 1127.18, r: 2254.36 UM TTTSOLUTION 5: 15 365(sub) 744(all), hR( 9, 8) 7.37 7.36 36.16 90.00 90.14 120.14 pr: 565.17, r: 1695.50 Peak table: 500(sub) 1258(all) Best cell: 409 indexed, Niggli cF( 1,12): 10.40 10.41 10.44 90.13 90.08 90.18 prim: 282.56, red: 1130.22 UM TTTSOLUTION 1: 16 409(sub) 928(all), cF( 1,12) 10.40 10.41 10.44 90.13 90.08 90.18 pr: 282.56, r: 1130.22 UM TTTSOLUTION 2: 17 324(sub) 947(all), hP(12, 9) 7.35 7.35 18.08 90.19 89.99 119.80 pr: 847.97, r: 847.97 UM TTTSOLUTION 3: 18 336(sub) 777(all), mI(27, 2) 18.07 7.35 22.10 90.07 105.60 90.01 pr: 1414.09, r: 2828.17 UM TTTSOLUTION 4: 19 342(sub) 769(all), tI(15, 7) 10.42 10.42 20.76 89.75 89.89 90.31 pr: 1127.18, r: 2254.36 UM TTTSOLUTION 5: 20 365(sub) 744(all), hR( 9, 8) 7.37 7.36 36.16 90.00 90.14 120.14 pr: 565.17, r: 1695.50 Peak table: 500(sub) 1258(all) Best cell: 409 indexed, Niggli cF( 1,12): 10.40 10.41 10.44 90.13 90.08 90.18 prim: 282.56, red: 1130.22 Make subset: 0.00015 Make T-vectors: 0.34903 Make unit cell: 0.46389 UM TTT INFO: Volume check Primitive unit cell refinement volume check UB fit with 1023 obs out of 1258 (total:1258,skipped:0) (81.32%) UB - matrix: -0.044477 -0.087901 0.058107 ( 0.000046 0.000045 0.000043 ) 0.093672 -0.061841 -0.067615 ( 0.000037 0.000036 0.000034 ) 0.056164 -0.048478 0.077048 ( 0.000035 0.000034 0.000033 ) M - matrix: 0.013907 -0.004606 -0.004591 ( 0.000009 0.000007 0.000006 ) -0.004606 0.013901 -0.004661 ( 0.000007 0.000010 0.000006 ) -0.004591 -0.004661 0.013885 ( 0.000006 0.000006 0.000008 ) unit cell: 7.345(3) 7.361(3) 7.362(3) 60.02(4) 60.22(4) 60.18(4) V = 282.3(2) UB fit with 1023 obs out of 1258 (total:1258,skipped:0) (81.32%) UB - matrix: -0.044464 -0.087903 0.058056 ( 0.000045 0.000044 0.000042 ) 0.093699 -0.061798 -0.067684 ( 0.000038 0.000036 0.000035 ) 0.056174 -0.048511 0.077040 ( 0.000036 0.000034 0.000033 ) M - matrix: 0.013912 -0.004607 -0.004596 ( 0.000009 0.000007 0.000006 ) -0.004607 0.013899 -0.004658 ( 0.000007 0.000010 0.000006 ) -0.004596 -0.004658 0.013887 ( 0.000006 0.000006 0.000008 ) unit cell: 7.344(3) 7.361(3) 7.362(3) 60.03(4) 60.20(4) 60.18(4) V = 282.3(2) UB fit with 1024 obs out of 1258 (total:1258,skipped:0) (81.40%) UB - matrix: -0.044452 -0.087902 0.058022 ( 0.000046 0.000044 0.000042 ) 0.093726 -0.061779 -0.067730 ( 0.000037 0.000036 0.000035 ) 0.056176 -0.048520 0.077029 ( 0.000036 0.000034 0.000033 ) M - matrix: 0.013916 -0.004609 -0.004600 ( 0.000009 0.000007 0.000006 ) -0.004609 0.013898 -0.004653 ( 0.000007 0.000010 0.000006 ) -0.004600 -0.004653 0.013887 ( 0.000006 0.000006 0.000008 ) unit cell: 7.344(3) 7.361(3) 7.362(3) 60.04(4) 60.19(4) 60.17(4) V = 282.3(2) UM TTT INFO: No smaller volume found Primitive unit cell refinement UB fit with 1023 obs out of 1258 (total:1258,skipped:0) (81.32%) UB - matrix: -0.044477 -0.087901 0.058107 ( 0.000046 0.000045 0.000043 ) 0.093672 -0.061841 -0.067615 ( 0.000037 0.000036 0.000034 ) 0.056164 -0.048478 0.077048 ( 0.000035 0.000034 0.000033 ) M - matrix: 0.013907 -0.004606 -0.004591 ( 0.000009 0.000007 0.000006 ) -0.004606 0.013901 -0.004661 ( 0.000007 0.000010 0.000006 ) -0.004591 -0.004661 0.013885 ( 0.000006 0.000006 0.000008 ) unit cell: 7.345(3) 7.361(3) 7.362(3) 60.02(4) 60.22(4) 60.18(4) V = 282.3(2) No constraint UB - matrix: 0.006815 -0.066140 -0.014949 ( 0.000018 0.000017 0.000019 ) 0.013012 0.015910 -0.064730 ( 0.000017 0.000016 0.000018 ) 0.066583 0.003875 0.014314 ( 0.000019 0.000018 0.000020 ) M - matrix: 0.004649 0.000014 0.000009 ( 0.000003 0.000002 0.000002 ) 0.000014 0.004643 0.000014 ( 0.000002 0.000002 0.000002 ) 0.000009 0.000014 0.004618 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.006815 -0.066140 -0.014949 ( 0.000018 0.000017 0.000019 ) 0.013012 0.015910 -0.064730 ( 0.000017 0.000016 0.000018 ) 0.066583 0.003875 0.014314 ( 0.000019 0.000018 0.000020 ) M - matrix: 0.004637 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004637 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004637 ( 0.000000 0.000000 0.000001 ) UB fit with 926 obs out of 1258 (total:1258,skipped:0) (73.61%) unit cell: 10.403(3) 10.410(3) 10.437(3) 90.18(2) 90.11(2) 90.18(2) V = 1130.3(5) unit cell: 10.4166(10) 10.4166(10) 10.4166(10) 90.0 90.0 90.0 V = 1130.27(19) AUTO INFO: Dirax ended... LAMBDA HALF REJECTION: Number of processed reflections: 835 Number of skipped reflections, because of (potential) lambda half effect: 158 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 1566411297! 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: 1 387(sub) 947(all), tP(11, 6) 7.35 7.36 10.43 89.91 89.99 89.92 pr: 564.72, r: 564.72 UM TTTSOLUTION 2: 2 406(sub) 869(all), cF( 1,12) 10.37 10.44 10.43 89.99 89.94 90.10 pr: 282.16, r: 1128.65 UM TTTSOLUTION 3: 3 340(sub) 831(all), oI(42, 4) 7.36 10.42 22.12 90.00 90.08 90.18 pr: 847.87, r: 1695.75 UM TTTSOLUTION 4: 4 336(sub) 788(all), tI(15, 7) 10.41 10.42 20.83 89.99 89.95 90.19 pr: 1130.24, r: 2260.48 Peak table: 500(sub) 1199(all) Best cell: 387 indexed, Niggli tP(11, 6): 7.35 7.36 10.43 89.91 89.99 89.92 prim: 564.72, red: 564.72 UM TTTSOLUTION 1: 5 387(sub) 947(all), tP(11, 6) 7.35 7.36 10.43 89.91 89.99 89.92 pr: 564.72, r: 564.72 UM TTTSOLUTION 2: 6 406(sub) 869(all), cF( 1,12) 10.37 10.44 10.43 89.99 89.94 90.10 pr: 282.16, r: 1128.65 UM TTTSOLUTION 3: 7 340(sub) 831(all), oI(42, 4) 7.36 10.42 22.12 90.00 90.08 90.18 pr: 847.87, r: 1695.75 UM TTTSOLUTION 4: 8 336(sub) 788(all), tI(15, 7) 10.41 10.42 20.83 89.99 89.95 90.19 pr: 1130.24, r: 2260.48 Peak table: 500(sub) 1199(all) Best cell: 387 indexed, Niggli tP(11, 6): 7.35 7.36 10.43 89.91 89.99 89.92 prim: 564.72, red: 564.72 UM TTTSOLUTION 1: 9 387(sub) 947(all), tP(11, 6) 7.35 7.36 10.43 89.91 89.99 89.92 pr: 564.72, r: 564.72 UM TTTSOLUTION 2: 10 313(sub) 899(all), hP(12, 9) 7.36 7.36 18.05 90.19 89.96 119.98 pr: 847.55, r: 847.55 UM TTTSOLUTION 3: 11 406(sub) 869(all), cF( 1,12) 10.37 10.44 10.43 89.99 89.94 90.10 pr: 282.16, r: 1128.65 UM TTTSOLUTION 4: 12 325(sub) 862(all), cP( 3,10) 10.41 10.42 10.43 90.17 90.00 90.24 pr: 1131.01, r: 1131.01 UM TTTSOLUTION 5: 13 306(sub) 675(all), mI(39, 2) 14.72 10.42 23.31 89.76 108.40 90.18 pr: 1696.74, r: 3393.48 Peak table: 500(sub) 1199(all) Best cell: 387 indexed, Niggli tP(11, 6): 7.35 7.36 10.43 89.91 89.99 89.92 prim: 564.72, red: 564.72 UM TTTSOLUTION 1: 14 406(sub) 869(all), cF( 1,12) 10.37 10.44 10.43 89.99 89.94 90.10 pr: 282.16, r: 1128.65 UM TTTSOLUTION 2: 15 313(sub) 899(all), hP(12, 9) 7.36 7.36 18.05 90.19 89.96 119.98 pr: 847.55, r: 847.55 UM TTTSOLUTION 3: 16 325(sub) 862(all), cP( 3,10) 10.41 10.42 10.43 90.17 90.00 90.24 pr: 1131.01, r: 1131.01 UM TTTSOLUTION 4: 17 353(sub) 727(all), hR( 9, 8) 7.35 7.38 36.10 89.97 90.01 119.99 pr: 565.33, r: 1695.98 UM TTTSOLUTION 5: 18 306(sub) 675(all), mI(39, 2) 14.72 10.42 23.31 89.76 108.40 90.18 pr: 1696.74, r: 3393.48 Peak table: 500(sub) 1199(all) Best cell: 406 indexed, Niggli cF( 1,12): 10.37 10.44 10.43 89.99 89.94 90.10 prim: 282.16, red: 1128.65 UM TTTSOLUTION 1: 19 406(sub) 869(all), cF( 1,12) 10.37 10.44 10.43 89.99 89.94 90.10 pr: 282.16, r: 1128.65 UM TTTSOLUTION 2: 20 313(sub) 899(all), hP(12, 9) 7.36 7.36 18.05 90.19 89.96 119.98 pr: 847.55, r: 847.55 UM TTTSOLUTION 3: 21 325(sub) 862(all), cP( 3,10) 10.41 10.42 10.43 90.17 90.00 90.24 pr: 1131.01, r: 1131.01 UM TTTSOLUTION 4: 22 353(sub) 727(all), hR( 9, 8) 7.35 7.38 36.10 89.97 90.01 119.99 pr: 565.33, r: 1695.98 UM TTTSOLUTION 5: 23 306(sub) 675(all), mI(39, 2) 14.72 10.42 23.31 89.76 108.40 90.18 pr: 1696.74, r: 3393.48 Peak table: 500(sub) 1199(all) Best cell: 406 indexed, Niggli cF( 1,12): 10.37 10.44 10.43 89.99 89.94 90.10 prim: 282.16, red: 1128.65 UM TTTSOLUTION 1: 24 406(sub) 869(all), cF( 1,12) 10.37 10.44 10.43 89.99 89.94 90.10 pr: 282.16, r: 1128.65 UM TTTSOLUTION 2: 25 313(sub) 899(all), hP(12, 9) 7.36 7.36 18.05 90.19 89.96 119.98 pr: 847.55, r: 847.55 UM TTTSOLUTION 3: 26 325(sub) 862(all), cP( 3,10) 10.41 10.42 10.43 90.17 90.00 90.24 pr: 1131.01, r: 1131.01 UM TTTSOLUTION 4: 27 353(sub) 727(all), hR( 9, 8) 7.35 7.38 36.10 89.97 90.01 119.99 pr: 565.33, r: 1695.98 UM TTTSOLUTION 5: 28 306(sub) 675(all), mI(39, 2) 14.72 10.42 23.31 89.76 108.40 90.18 pr: 1696.74, r: 3393.48 Peak table: 500(sub) 1199(all) Best cell: 406 indexed, Niggli cF( 1,12): 10.37 10.44 10.43 89.99 89.94 90.10 prim: 282.16, red: 1128.65 UM TTTSOLUTION 1: 29 406(sub) 869(all), cF( 1,12) 10.37 10.44 10.43 89.99 89.94 90.10 pr: 282.16, r: 1128.65 UM TTTSOLUTION 2: 30 313(sub) 899(all), hP(12, 9) 7.36 7.36 18.05 90.19 89.96 119.98 pr: 847.55, r: 847.55 UM TTTSOLUTION 3: 31 325(sub) 862(all), cP( 3,10) 10.41 10.42 10.43 90.17 90.00 90.24 pr: 1131.01, r: 1131.01 UM TTTSOLUTION 4: 32 353(sub) 727(all), hR( 9, 8) 7.35 7.38 36.10 89.97 90.01 119.99 pr: 565.33, r: 1695.98 UM TTTSOLUTION 5: 33 306(sub) 675(all), mI(39, 2) 14.72 10.42 23.31 89.76 108.40 90.18 pr: 1696.74, r: 3393.48 Peak table: 500(sub) 1199(all) Best cell: 406 indexed, Niggli cF( 1,12): 10.37 10.44 10.43 89.99 89.94 90.10 prim: 282.16, red: 1128.65 Make subset: 0.00014 Make T-vectors: 0.58268 Make unit cell: 0.86602 UM TTT INFO: Volume check Primitive unit cell refinement volume check UB fit with 974 obs out of 1199 (total:1258,skipped:59) (81.23%) UB - matrix: -0.058144 -0.013537 -0.087955 ( 0.000038 0.000047 0.000041 ) 0.067689 -0.026235 -0.061857 ( 0.000033 0.000041 0.000035 ) -0.077086 -0.132926 -0.048412 ( 0.000045 0.000056 0.000048 ) M - matrix: 0.013905 0.009258 0.004659 ( 0.000009 0.000008 0.000007 ) 0.009258 0.018541 0.009249 ( 0.000008 0.000015 0.000009 ) 0.004659 0.009249 0.013906 ( 0.000007 0.000009 0.000010 ) unit cell: 7.362(3) 7.349(3) 7.358(3) 119.82(5) 90.25(4) 119.87(5) V = 282.2(2) UB fit with 982 obs out of 1199 (total:1258,skipped:59) (81.90%) UB - matrix: -0.058076 -0.013609 -0.087965 ( 0.000038 0.000047 0.000040 ) 0.067691 -0.026103 -0.061805 ( 0.000033 0.000041 0.000035 ) -0.077026 -0.133084 -0.048472 ( 0.000045 0.000056 0.000048 ) M - matrix: 0.013888 0.009274 0.004659 ( 0.000009 0.000008 0.000007 ) 0.009274 0.018578 0.009261 ( 0.000008 0.000015 0.000009 ) 0.004659 0.009261 0.013907 ( 0.000007 0.000009 0.000010 ) unit cell: 7.372(3) 7.347(3) 7.359(3) 119.83(5) 90.22(3) 119.93(5) V = 282.3(2) UB fit with 980 obs out of 1199 (total:1258,skipped:59) (81.73%) UB - matrix: -0.058043 -0.013641 -0.087968 ( 0.000037 0.000046 0.000040 ) 0.067712 -0.026036 -0.061784 ( 0.000033 0.000041 0.000035 ) -0.077000 -0.133156 -0.048495 ( 0.000046 0.000057 0.000049 ) M - matrix: 0.013883 0.009282 0.004657 ( 0.000009 0.000008 0.000007 ) 0.009282 0.018595 0.009266 ( 0.000008 0.000015 0.000009 ) 0.004657 0.009266 0.013907 ( 0.000007 0.000009 0.000009 ) unit cell: 7.375(3) 7.346(3) 7.359(3) 119.83(5) 90.19(3) 119.96(5) V = 282.3(2) UM TTT INFO: No smaller volume found Primitive unit cell refinement UB fit with 974 obs out of 1199 (total:1258,skipped:59) (81.23%) UB - matrix: -0.058144 -0.013537 -0.087955 ( 0.000038 0.000047 0.000041 ) 0.067689 -0.026235 -0.061857 ( 0.000033 0.000041 0.000035 ) -0.077086 -0.132926 -0.048412 ( 0.000045 0.000056 0.000048 ) M - matrix: 0.013905 0.009258 0.004659 ( 0.000009 0.000008 0.000007 ) 0.009258 0.018541 0.009249 ( 0.000008 0.000015 0.000009 ) 0.004659 0.009249 0.013906 ( 0.000007 0.000009 0.000010 ) unit cell: 7.362(3) 7.349(3) 7.358(3) 119.82(5) 90.25(4) 119.87(5) V = 282.2(2) No constraint UB - matrix: 0.066198 0.014955 0.006776 ( 0.000018 0.000019 0.000019 ) -0.015989 0.064770 0.013078 ( 0.000015 0.000017 0.000016 ) -0.003807 -0.014357 0.066507 ( 0.000017 0.000018 0.000018 ) M - matrix: 0.004652 0.000009 -0.000014 ( 0.000002 0.000002 0.000002 ) 0.000009 0.004625 -0.000006 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000006 0.004640 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066198 0.014955 0.006776 ( 0.000018 0.000019 0.000019 ) -0.015989 0.064770 0.013078 ( 0.000015 0.000017 0.000016 ) -0.003807 -0.014357 0.066507 ( 0.000017 0.000018 0.000018 ) M - matrix: 0.004640 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004640 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004640 ( 0.000000 0.000000 0.000001 ) UB fit with 871 obs out of 1199 (total:1258,skipped:59) (72.64%) unit cell: 10.399(3) 10.430(3) 10.413(3) 89.92(2) 89.83(2) 90.11(2) V = 1129.4(5) unit cell: 10.4139(10) 10.4139(10) 10.4139(10) 90.0 90.0 90.0 V = 1129.36(18) AUTO INFO: Dirax ended... ******************************************************************************************************* Auto analyse stage: MODEL REFINEMENT (Wed Aug 21 14:14:59 2019) ******************************************************************************************************* UB fit with 926 obs out of 1258 (total:1258,skipped:0) (73.61%) UB - matrix: 0.066136 0.014997 0.006790 ( 0.000017 0.000018 0.000018 ) -0.015974 0.064761 0.013060 ( 0.000015 0.000017 0.000016 ) -0.003841 -0.014352 0.066549 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004644 0.000012 -0.000015 ( 0.000002 0.000002 0.000002 ) 0.000012 0.004625 -0.000007 ( 0.000002 0.000002 0.000002 ) -0.000015 -0.000007 0.004645 ( 0.000002 0.000002 0.000003 ) unit cell: 10.409(2) 10.430(3) 10.407(3) 89.91(2) 89.81(2) 90.15(2) V = 1129.8(5) OTKP changes: 161 2 4 5 Cycle 1 - Res: 0.035304, da=0.031726, sx=0.003321, sy=0.003978, h=0.008823, k=0.009074, l=0.007269, LM=0.000000 Cycle 2 - Res: 0.033203, da=0.029784, sx=0.003152, sy=0.003774, h=0.008364, k=0.008613, l=0.006860, LM=0.000000 Cycle 3 - Res: 0.033198, da=0.029778, sx=0.003152, sy=0.003774, h=0.008364, k=0.008613, l=0.006860, LM=0.000000 Cycle 4 - Res: 0.033198, da=0.029778, sx=0.003152, sy=0.003774, h=0.008364, k=0.008613, l=0.006860, LM=0.000000 Model change (all parameters): Omega Offset 0.085649 0.150322 0.0646737 6.19654e-006 1 Kappa Offset -0.112630 -0.112630 0 0 0 Phi Offset 0.000000 0.000000 0 0 0 Alpha Value 50.029020 50.029020 0 0 0 Beta Value -0.000700 -0.000700 0 0 0 Theta Offset -0.142281 -0.208114 -0.0658327 8.47511e-006 1 Det. D. Scale 53.098497 53.156426 0.0579293 8.66832e-006 1 Det. Offset X 1028.463598 1027.313833 -1.14976 0.000182337 1 Det. Offset Y 1025.668784 1024.567410 -1.10137 0.000206528 1 Det. Rot. X 0.597782 0.584715 -0.0130664 4.00596e-006 1 Det. Rot. Y 0.099478 0.176106 0.0766287 8.94712e-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 0.183671 0.215334 0.0316631 4.84023e-006 1 Beam. Rot. Z 0.000000 0.000000 0 0 0 Cryst. Rot. X 12.193884 12.256151 0.0622669 4.94635e-006 1 Cryst. Rot. Y -3.231474 -3.077073 0.154401 4.72326e-006 1 Cryst. Rot. Z 13.579041 13.663382 0.0843404 6.72011e-006 1 Rec. latt. a* 0.096075 0.096007 -6.82232e-005 1.25639e-008 1 Rec. latt. b* 0.095878 0.095875 -2.65864e-006 1.24059e-008 1 Rec. latt. c* 0.096091 0.095933 -0.000158216 1.21827e-008 1 Rec. latt. al* 90.092435 90.065166 -0.0272694 6.10724e-006 1 Rec. latt. be* 90.187667 90.142273 -0.0453938 6.31616e-006 1 Rec. latt. ga* 89.845818 89.891115 0.0452975 6.24761e-006 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: 0.066051 0.015040 0.006752 ( 0.000016 0.000018 0.000017 ) -0.016016 0.064730 0.013114 ( 0.000014 0.000016 0.000015 ) -0.003747 -0.014413 0.066487 ( 0.000016 0.000018 0.000017 ) M - matrix: 0.004633 0.000011 -0.000013 ( 0.000002 0.000002 0.000002 ) 0.000011 0.004624 -0.000008 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000008 0.004638 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066051 0.015040 0.006752 ( 0.000016 0.000018 0.000017 ) -0.016016 0.064730 0.013114 ( 0.000014 0.000016 0.000015 ) -0.003747 -0.014413 0.066487 ( 0.000016 0.000018 0.000017 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000001 ) UB fit with 928 obs out of 1258 (total:1258,skipped:0) (73.77%) unit cell: 10.420(2) 10.431(2) 10.415(3) 89.90(2) 89.84(2) 90.132(19) V = 1132.1(5) unit cell: 10.4222(10) 10.4222(10) 10.4222(10) 90.0 90.0 90.0 V = 1132.07(18) No constraint UB - matrix: 0.066037 0.015028 0.006779 ( 0.000016 0.000018 0.000017 ) -0.015984 0.064722 0.013089 ( 0.000015 0.000016 0.000016 ) -0.003809 -0.014405 0.066519 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004631 0.000013 -0.000015 ( 0.000002 0.000002 0.000002 ) 0.000013 0.004622 -0.000009 ( 0.000002 0.000002 0.000002 ) -0.000015 -0.000009 0.004642 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066037 0.015028 0.006779 ( 0.000016 0.000018 0.000017 ) -0.015984 0.064722 0.013089 ( 0.000015 0.000016 0.000016 ) -0.003809 -0.014405 0.066519 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000001 ) UB fit with 926 obs out of 1258 (total:1258,skipped:0) (73.61%) unit cell: 10.423(2) 10.433(2) 10.411(3) 89.89(2) 89.82(2) 90.16(2) V = 1132.1(5) unit cell: 10.4222(10) 10.4222(10) 10.4222(10) 90.0 90.0 90.0 V = 1132.08(19) No constraint UB - matrix: 0.066037 0.015023 0.006790 ( 0.000016 0.000018 0.000017 ) -0.015957 0.064710 0.013079 ( 0.000015 0.000017 0.000016 ) -0.003845 -0.014390 0.066536 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004630 0.000015 -0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.004620 -0.000009 ( 0.000002 0.000002 0.000002 ) -0.000016 -0.000009 0.004644 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066037 0.015023 0.006790 ( 0.000016 0.000018 0.000017 ) -0.015957 0.064710 0.013079 ( 0.000015 0.000017 0.000016 ) -0.003845 -0.014390 0.066536 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 929 obs out of 1258 (total:1258,skipped:0) (73.85%) unit cell: 10.424(2) 10.435(2) 10.408(3) 89.89(2) 89.80(2) 90.18(2) V = 1132.2(5) unit cell: 10.4224(10) 10.4224(10) 10.4224(10) 90.0 90.0 90.0 V = 1132.16(19) ******************************************************************************************************* Auto analyse stage: BRAVAIS LATTICE FINDING (Wed Aug 21 14:14:59 2019) ******************************************************************************************************* Bravais lattice type: F Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" 2250 peak locations are merged to 1258 profiles (Parameters: ofix = 2.00, otan(th) = 0.00) We have put 1258 unindexed peaks to the CrysAlis peak table (1258 with profile info) No constraint UB - matrix: 0.066039 0.015016 0.006798 ( 0.000016 0.000018 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000015 0.000017 0.000016 ) -0.003867 -0.014380 0.066544 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004630 0.000017 -0.000017 ( 0.000002 0.000002 0.000002 ) 0.000017 0.004618 -0.000009 ( 0.000002 0.000002 0.000002 ) -0.000017 -0.000009 0.004645 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066039 0.015016 0.006798 ( 0.000016 0.000018 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000015 0.000017 0.000016 ) -0.003867 -0.014380 0.066544 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 933 obs out of 1258 (total:1258,skipped:0) (74.17%) unit cell: 10.424(2) 10.438(3) 10.407(3) 89.89(2) 89.80(2) 90.20(2) V = 1132.4(5) unit cell: 10.4231(10) 10.4231(10) 10.4231(10) 90.0 90.0 90.0 V = 1132.38(19) -------------------EXPERIMENT TAB SUMMARY------------------- CELL Niggli 1 cubic F 72.644 %(871/1258) 10.399(3) 10.430(3) 10.413(3) 89.92(2) 89.83(2) 90.11(2) V = 1129.4(5) ------------------------------------------------------------ AUTO INFO: Finished at Wed Aug 21 14:14:59 2019 DC PROFFIT INFO: Meta algorithm started DELETE INFO: Deleting rpi files... (D:\Data\xs2212a\tmp\xs2212a_proffitpea*.rpi) DELETE INFO: Deleting tab files... (D:\Data\xs2212a\tmp\xs2212a_proffitpea*.tab) DELETE INFO: Deleting tabbin files... (D:\Data\xs2212a\tmp\xs2212a_proffitpea*.tabbin) DELETE INFO: Deleting rrpprof files... (D:\Data\xs2212a\tmp\xs2212a*.rrpprof) DELETE INFO: Deleting rrpprofinfo files... (D:\Data\xs2212a\tmp\xs2212a*.rrpprofinfo) DELETE INFO: Deleting bbm files... (D:\Data\xs2212a\tmp\xs2212a*.bbm) DELETE INFO: Deleting pcorr files... (D:\Data\xs2212a\tmp\xs2212a*.pcorr) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\tmp\xs2212a*.dat) DELETE INFO: Deleting ppc2 files... (D:\Data\xs2212a\tmp\xs2212a*.ppc2) DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:15:00 2019) ID: 3668; threads 40; handles 811; mem 514192.00 (1204692.00)kB; time: 1w 5d 0h 25m 48s MEMORY INFO: Memory PF:238.0, Ph:560.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.2,peak PF: 700.2, WS: 469.6, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:240.0, Ph:561.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.0,peak PF: 700.2, WS: 471.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:15:00 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000016 0.000018 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000015 0.000017 0.000016 ) -0.003867 -0.014380 0.066544 ( 0.000017 0.000019 0.000018 ) 10.42433 ( 0.00245 ) 10.43788 ( 0.00259 ) 10.40727 ( 0.00279 ) 89.88512 ( 0.02101 ) 89.79539 ( 0.02037 ) 90.20497 ( 0.01966 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 cF Cross checking gral lattice... 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(D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:15:01 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000016 0.000018 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000015 0.000017 0.000016 ) -0.003867 -0.014380 0.066544 ( 0.000017 0.000019 0.000018 ) M - matrix: 0.004630 0.000017 -0.000017 ( 0.000002 0.000002 0.000002 ) 0.000017 0.004618 -0.000009 ( 0.000002 0.000002 0.000002 ) -0.000017 -0.000009 0.004645 ( 0.000002 0.000002 0.000002 ) unit cell: 10.424(2) 10.438(3) 10.407(3) 89.89(2) 89.80(2) 90.20(2) V = 1132.4(5) unit cell: 10.4231(10) 10.4231(10) 10.4231(10) 90.0 90.0 90.0 V = 1132.38(19) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.938 ( 0.170) | 0.923 ( 0.398) | 1.01- 0.88 | 22 | 0.957 ( 0.073) | 1.004 ( 0.124) | 1.180 ( 0.493) | 0.88- 0.79 | 22 | 0.985 ( 0.059) | 1.028 ( 0.140) | 1.234 ( 0.387) | 0.79- 0.70 | 22 | 0.984 ( 0.041) | 0.962 ( 0.107) | 1.276 ( 0.475) | 0.70- 0.63 | 22 | 0.943 ( 0.038) | 0.917 ( 0.081) | 1.311 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 220 | 0.933 ( 0.193) | 0.943 ( 0.158) | 1.113 ( 0.914) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.87 | 25 | 0.945 ( 0.067) | 0.936 ( 0.094) | 1.074 ( 0.403) | 0.86- 0.73 | 25 | 0.958 ( 0.050) | 0.919 ( 0.091) | 1.335 ( 0.450) | 0.73- 0.63 | 29 | 0.929 ( 0.037) | 0.880 ( 0.095) | 1.340 ( 0.463) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 254 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.061 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=72, end=96, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_5_72.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_72.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_5_72.rpb PROFFITPEAK info: 492 peaks in the peak location table UB fit with 225 obs out of 276 (total:277,skipped:1) (81.52%) UB - matrix: 0.066033 0.015276 0.006421 ( 0.000039 0.000032 0.000026 ) -0.016273 0.064758 0.013275 ( 0.000039 0.000031 0.000026 ) -0.003219 -0.014524 0.066417 ( 0.000040 0.000032 0.000026 ) M - matrix: 0.004636 0.000002 -0.000006 ( 0.000005 0.000003 0.000003 ) 0.000002 0.004638 -0.000007 ( 0.000003 0.000004 0.000003 ) -0.000006 -0.000007 0.004629 ( 0.000003 0.000003 0.000004 ) unit cell: 10.418(6) 10.415(5) 10.426(4) 89.92(3) 89.93(4) 90.02(4) V = 1131.2(9) UB fit with 225 obs out of 276 (total:277,skipped:1) (81.52%) UB - matrix: 0.066033 0.015276 0.006421 ( 0.000039 0.000032 0.000026 ) -0.016273 0.064758 0.013275 ( 0.000039 0.000031 0.000026 ) -0.003219 -0.014524 0.066417 ( 0.000040 0.000032 0.000026 ) M - matrix: 0.004636 0.000002 -0.000006 ( 0.000005 0.000003 0.000003 ) 0.000002 0.004638 -0.000007 ( 0.000003 0.000004 0.000003 ) -0.000006 -0.000007 0.004629 ( 0.000003 0.000003 0.000004 ) unit cell: 10.418(6) 10.415(5) 10.426(4) 89.92(3) 89.93(4) 90.02(4) V = 1131.2(9) OTKP changes: 92 1 1 1 OTKP changes: 92 1 1 1 OTKP changes: 92 1 1 1 No constraint UB - matrix: 0.065996 0.015416 0.006306 ( 0.000035 0.000027 0.000025 ) -0.016332 0.064721 0.013339 ( 0.000032 0.000025 0.000023 ) -0.002934 -0.014609 0.066395 ( 0.000029 0.000022 0.000020 ) M - matrix: 0.004631 0.000003 0.000004 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004640 -0.000009 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000009 0.004626 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.065996 0.015416 0.006306 ( 0.000035 0.000027 0.000025 ) -0.016332 0.064721 0.013339 ( 0.000032 0.000025 0.000023 ) -0.002934 -0.014609 0.066395 ( 0.000029 0.000022 0.000020 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000001 ) UB fit with 252 obs out of 276 (total:277,skipped:1) (91.30%) unit cell: 10.423(5) 10.413(4) 10.429(3) 89.88(3) 90.04(3) 90.04(3) V = 1131.9(8) unit cell: 10.4216(11) 10.4216(11) 10.4216(11) 90.0 90.0 90.0 V = 1131.9(2) UB fit with 252 obs out of 276 (total:277,skipped:1) (91.30%) UB - matrix: 0.065996 0.015416 0.006306 ( 0.000035 0.000027 0.000025 ) -0.016332 0.064721 0.013339 ( 0.000032 0.000025 0.000023 ) -0.002934 -0.014609 0.066395 ( 0.000029 0.000022 0.000020 ) M - matrix: 0.004631 0.000003 0.000004 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004640 -0.000009 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000009 0.004626 ( 0.000003 0.000002 0.000003 ) unit cell: 10.423(5) 10.413(4) 10.429(3) 89.88(3) 90.04(3) 90.04(3) V = 1131.9(8) OTKP changes: 92 1 1 1 OTKP changes: 92 1 1 1 OTKP changes: 92 1 1 1 OTKP changes: 92 1 1 1 OTKP changes: 92 1 1 1 OTKP changes: 92 1 1 1 277 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Run 5 Omega scan: (-6.000 - 90.000,96 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1233 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065996 0.015416 0.006306 ( 0.000035 0.000027 0.000025 ) -0.016332 0.064721 0.013339 ( 0.000032 0.000025 0.000023 ) -0.002934 -0.014609 0.066395 ( 0.000029 0.000022 0.000020 ) M - matrix: 0.004631 0.000003 0.000004 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004640 -0.000009 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000009 0.004626 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.065996 0.015416 0.006306 ( 0.000035 0.000027 0.000025 ) -0.016332 0.064721 0.013339 ( 0.000032 0.000025 0.000023 ) -0.002934 -0.014609 0.066395 ( 0.000029 0.000022 0.000020 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000001 ) UB fit with 252 obs out of 276 (total:277,skipped:1) (91.30%) unit cell: 10.423(5) 10.413(4) 10.429(3) 89.88(3) 90.04(3) 90.04(3) V = 1131.9(8) unit cell: 10.4216(11) 10.4216(11) 10.4216(11) 90.0 90.0 90.0 V = 1131.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 276 (total:277,skipped:1) (91.67%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=72, end=96, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_72.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_72.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_72.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.36 | 25 | 0.899 ( 0.102) | 0.910 ( 0.132) | 0.832 ( 0.204) | 2.13- 1.76 | 25 | 0.903 ( 0.130) | 0.999 ( 0.377) | 0.979 ( 0.586) | 1.75- 1.56 | 25 | 0.951 ( 0.116) | 0.959 ( 0.148) | 0.952 ( 0.377) | 1.56- 1.35 | 25 | 0.962 ( 0.102) | 0.972 ( 0.156) | 0.828 ( 0.310) | 1.35- 1.19 | 25 | 0.939 ( 0.087) | 0.974 ( 0.152) | 0.733 ( 0.259) | 1.19- 1.06 | 25 | 0.995 ( 0.061) | 1.045 ( 0.100) | 0.893 ( 0.352) | 1.06- 0.92 | 25 | 1.013 ( 0.076) | 1.079 ( 0.115) | 0.959 ( 0.390) | 0.92- 0.87 | 25 | 1.007 ( 0.062) | 0.996 ( 0.109) | 1.092 ( 0.371) | 0.87- 0.73 | 25 | 1.046 ( 0.052) | 1.025 ( 0.140) | 1.200 ( 0.444) | 0.73- 0.63 | 27 | 1.004 ( 0.040) | 1.018 ( 0.119) | 1.037 ( 0.317) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 252 | 0.972 ( 0.099) | 0.998 ( 0.178) | 0.951 ( 0.396) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 251 obs out of 252 (total:252,skipped:0) (99.60%) UB - matrix: 0.066026 0.015414 0.006417 ( 0.000020 0.000015 0.000015 ) -0.016403 0.064853 0.013475 ( 0.000024 0.000018 0.000018 ) -0.002799 -0.014640 0.066439 ( 0.000019 0.000015 0.000015 ) M - matrix: 0.004636 -0.000005 0.000017 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004658 0.000000 ( 0.000002 0.000002 0.000002 ) 0.000017 0.000000 0.004637 ( 0.000002 0.000002 0.000002 ) unit cell: 10.417(3) 10.393(3) 10.416(2) 90.00(2) 90.21(2) 89.94(2) V = 1127.7(5) OTKP changes: 251 1 1 1 OTKP changes: 251 1 1 1 OTKP changes: 251 1 1 1 No constraint UB - matrix: 0.065955 0.015315 0.006308 ( 0.000018 0.000013 0.000013 ) -0.016318 0.064768 0.013386 ( 0.000019 0.000014 0.000014 ) -0.002859 -0.014636 0.066457 ( 0.000017 0.000013 0.000013 ) M - matrix: 0.004625 -0.000005 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000005 0.004644 -0.000009 ( 0.000002 0.000002 0.000001 ) 0.000008 -0.000009 0.004635 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065955 0.015315 0.006308 ( 0.000018 0.000013 0.000013 ) -0.016318 0.064768 0.013386 ( 0.000019 0.000014 0.000014 ) -0.002859 -0.014636 0.066457 ( 0.000017 0.000013 0.000013 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 251 obs out of 252 (total:252,skipped:0) (99.60%) unit cell: 10.430(3) 10.409(2) 10.418(2) 89.888(17) 90.094(18) 89.939(19) V = 1131.0(4) unit cell: 10.4190(6) 10.4190(6) 10.4190(6) 90.0 90.0 90.0 V = 1131.05(12) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 90.000,96 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1231 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065955 0.015315 0.006308 ( 0.000018 0.000013 0.000013 ) -0.016318 0.064768 0.013386 ( 0.000019 0.000014 0.000014 ) -0.002859 -0.014636 0.066457 ( 0.000017 0.000013 0.000013 ) M - matrix: 0.004625 -0.000005 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000005 0.004644 -0.000009 ( 0.000002 0.000002 0.000001 ) 0.000008 -0.000009 0.004635 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065955 0.015315 0.006308 ( 0.000018 0.000013 0.000013 ) -0.016318 0.064768 0.013386 ( 0.000019 0.000014 0.000014 ) -0.002859 -0.014636 0.066457 ( 0.000017 0.000013 0.000013 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 251 obs out of 252 (total:252,skipped:0) (99.60%) unit cell: 10.430(3) 10.409(2) 10.418(2) 89.888(17) 90.094(18) 89.939(19) V = 1131.0(4) unit cell: 10.4190(6) 10.4190(6) 10.4190(6) 90.0 90.0 90.0 V = 1131.05(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 251 obs out of 252 (total:252,skipped:0) (99.60%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=72, end=96, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_72.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_72.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_72.rpb 0 of 251 peaks identified as outliers and rejected 251 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 251 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 251 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.13 | 25 | 0.902 ( 0.100) | 0.921 ( 0.136) | 0.802 ( 0.166) | 2.12- 1.76 | 25 | 0.912 ( 0.131) | 1.034 ( 0.481) | 0.950 ( 0.485) | 1.76- 1.57 | 25 | 0.972 ( 0.116) | 0.990 ( 0.146) | 1.010 ( 0.426) | 1.50- 1.35 | 25 | 0.959 ( 0.095) | 0.971 ( 0.158) | 0.764 ( 0.290) | 1.35- 1.19 | 25 | 0.937 ( 0.106) | 0.965 ( 0.158) | 0.791 ( 0.386) | 1.19- 1.06 | 25 | 0.988 ( 0.063) | 1.032 ( 0.094) | 0.862 ( 0.281) | 1.06- 0.92 | 25 | 1.011 ( 0.074) | 1.075 ( 0.118) | 0.976 ( 0.391) | 0.92- 0.87 | 25 | 1.009 ( 0.061) | 1.020 ( 0.119) | 1.091 ( 0.388) | 0.87- 0.73 | 25 | 1.043 ( 0.054) | 1.023 ( 0.133) | 1.231 ( 0.477) | 0.73- 0.63 | 26 | 1.004 ( 0.041) | 1.019 ( 0.125) | 1.040 ( 0.323) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 251 | 0.974 ( 0.099) | 1.005 ( 0.202) | 0.952 ( 0.399) | 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- 9.9 | 119 | 0.988 ( 0.040) | 1.032 ( 0.066) | 1.102 ( 0.466) | 10.0-14.6 | 119 | 0.993 ( 0.046) | 1.047 ( 0.069) | 1.120 ( 0.544) | 14.6-18.7 | 119 | 0.996 ( 0.194) | 1.033 ( 0.101) | 1.145 ( 1.020) | 18.8-23.4 | 119 | 0.969 ( 0.059) | 1.013 ( 0.083) | 0.925 ( 0.413) | 23.4-27.0 | 119 | 0.967 ( 0.063) | 1.000 ( 0.096) | 0.991 ( 0.454) | 27.0-32.1 | 119 | 0.944 ( 0.080) | 0.959 ( 0.104) | 0.956 ( 0.454) | 32.1-36.3 | 119 | 0.927 ( 0.159) | 0.925 ( 0.145) | 1.047 ( 0.664) | 36.3-38.9 | 119 | 0.886 ( 0.102) | 0.888 ( 0.262) | 1.046 ( 0.503) | 38.9-42.0 | 119 | 0.900 ( 0.098) | 0.845 ( 0.130) | 1.022 ( 0.466) | 42.0-50.1 | 115 | 0.865 ( 0.123) | 0.798 ( 0.141) | 0.905 ( 0.426) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1186 | 0.944 ( 0.116) | 0.955 ( 0.155) | 1.026 ( 0.574) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.14 e2 dimension: a=-0.0067 b=1.23 e3 dimension: a=0.0006 b=1.09 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 4895 Maximum peak integral for reflections I/sig<= 100 - raw: 458067 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563569 PROFFITPEAK - Finished at Wed Aug 21 14:15:16 2019 PROFFITMAIN - Started at Wed Aug 21 14:15:16 2019 OTKP changes: 944 2 4 5 OTKP changes: 944 2 4 5 OTKP changes: 944 2 4 5 No constraint UB - matrix: 0.066026 0.014999 0.006785 ( 0.000014 0.000016 0.000015 ) -0.016036 0.064671 0.013086 ( 0.000014 0.000016 0.000015 ) -0.003780 -0.014368 0.066559 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004631 0.000008 -0.000013 ( 0.000002 0.000001 0.000001 ) 0.000008 0.004614 -0.000008 ( 0.000001 0.000002 0.000002 ) -0.000013 -0.000008 0.004647 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: 0.066026 0.014999 0.006785 ( 0.000014 0.000016 0.000015 ) -0.016036 0.064671 0.013086 ( 0.000014 0.000016 0.000015 ) -0.003780 -0.014368 0.066559 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 952 obs out of 1186 (total:1186,skipped:0) (80.27%) unit cell: 10.423(2) 10.442(2) 10.405(2) 89.899(19) 89.834(18) 90.094(18) V = 1132.5(4) unit cell: 10.4234(8) 10.4234(8) 10.4234(8) 90.0 90.0 90.0 V = 1132.47(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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 187 obs out of 220 (total:220,skipped:0) (85.00%) UB - matrix: 0.066500 0.011702 0.008960 ( 0.000032 0.000043 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000030 0.000040 0.000034 ) -0.006052 -0.013931 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.60(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004603 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 220 (total:220,skipped:0) (85.91%) unit cell: 10.406(5) 10.502(6) 10.456(6) 90.61(5) 90.19(4) 89.64(4) V = 1143(1) unit cell: 10.4543(19) 10.4543(19) 10.4543(19) 90.0 90.0 90.0 V = 1142.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 220 (total:220,skipped:0) (92.27%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004644 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 220 (total:220,skipped:0) (93.64%) unit cell: 10.409(4) 10.492(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1140.0(9) unit cell: 10.4466(13) 10.4466(13) 10.4466(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.066336 0.014186 0.006779 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064704 0.012861 ( 0.000017 0.000022 0.000023 ) -0.004076 -0.014197 0.066901 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.393(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4047(5) 10.4047(5) 10.4047(5) 90.0 90.0 90.0 V = 1126.40(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065848 0.015169 0.006782 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064725 0.013269 ( 0.000016 0.000011 0.000016 ) -0.003665 -0.014493 0.066462 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004608 0.000012 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000012 0.004629 -0.000002 ( 0.000001 0.000002 0.000001 ) -0.000010 -0.000002 0.004639 ( 0.000002 0.000001 0.000003 ) unit cell: 10.449(3) 10.4248(19) 10.414(3) 89.981(18) 89.87(2) 90.147(18) V = 1134.4(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065818 0.015151 0.006803 ( 0.000019 0.000013 0.000019 ) -0.016051 0.064729 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003671 -0.014466 0.066438 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004603 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004629 0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 0.000000 0.004636 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065818 0.015151 0.006803 ( 0.000019 0.000013 0.000019 ) -0.016051 0.064729 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003671 -0.014466 0.066438 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.455(3) 10.4256(19) 10.417(3) 90.001(19) 89.89(2) 90.141(18) V = 1135.4(5) unit cell: 10.4325(6) 10.4325(6) 10.4325(6) 90.0 90.0 90.0 V = 1135.43(11) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.183) HKL list info: 1274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065818 0.015151 0.006803 ( 0.000019 0.000013 0.000019 ) -0.016051 0.064729 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003671 -0.014466 0.066438 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004603 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004629 0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 0.000000 0.004636 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065818 0.015151 0.006803 ( 0.000019 0.000013 0.000019 ) -0.016051 0.064729 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003671 -0.014466 0.066438 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.455(3) 10.4256(19) 10.417(3) 90.001(19) 89.89(2) 90.141(18) V = 1135.4(5) unit cell: 10.4325(6) 10.4325(6) 10.4325(6) 90.0 90.0 90.0 V = 1135.43(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065818 0.015151 0.006803 ( 0.000019 0.000013 0.000019 ) -0.016051 0.064729 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003671 -0.014466 0.066438 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004603 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004629 0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 0.000000 0.004636 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065818 0.015151 0.006803 ( 0.000019 0.000013 0.000019 ) -0.016051 0.064729 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003671 -0.014466 0.066438 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.455(3) 10.4256(19) 10.417(3) 90.001(19) 89.89(2) 90.141(18) V = 1135.4(5) unit cell: 10.4325(6) 10.4325(6) 10.4325(6) 90.0 90.0 90.0 V = 1135.43(11) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 221 obs out of 222 (total:222,skipped:0) (99.55%) UB - matrix: 0.066071 0.015212 0.006573 ( 0.000013 0.000018 0.000015 ) -0.016350 0.064698 0.012953 ( 0.000013 0.000017 0.000015 ) -0.003389 -0.014178 0.066467 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004644 -0.000005 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004629 ( 0.000001 0.000001 0.000002 ) unit cell: 10.408(2) 10.437(2) 10.4255(18) 89.946(17) 89.966(16) 89.943(18) V = 1132.6(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066037 0.015190 0.006553 ( 0.000013 0.000018 0.000015 ) -0.016303 0.064671 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003375 -0.014171 0.066477 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004638 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004614 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004630 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066037 0.015190 0.006553 ( 0.000013 0.000018 0.000015 ) -0.016303 0.064671 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003375 -0.014171 0.066477 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.415(2) 10.442(2) 10.4239(18) 89.948(16) 89.964(16) 89.957(18) V = 1133.7(4) unit cell: 10.4270(5) 10.4270(5) 10.4270(5) 90.0 90.0 90.0 V = 1133.66(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.183) HKL list info: 1300 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066037 0.015190 0.006553 ( 0.000013 0.000018 0.000015 ) -0.016303 0.064671 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003375 -0.014171 0.066477 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004638 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004614 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004630 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066037 0.015190 0.006553 ( 0.000013 0.000018 0.000015 ) -0.016303 0.064671 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003375 -0.014171 0.066477 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.415(2) 10.442(2) 10.4239(18) 89.948(16) 89.964(16) 89.957(18) V = 1133.7(4) unit cell: 10.4270(5) 10.4270(5) 10.4270(5) 90.0 90.0 90.0 V = 1133.66(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068089 -0.000049 -0.000032 ( 0.000011 0.000015 0.000012 ) 0.000002 0.067941 -0.000048 ( 0.000013 0.000018 0.000015 ) 0.000006 0.000008 0.068046 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004636 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004616 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004630 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068089 -0.000049 -0.000032 ( 0.000011 0.000015 0.000012 ) 0.000002 0.067941 -0.000048 ( 0.000013 0.000018 0.000015 ) 0.000006 0.000008 0.068046 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.4172(17) 10.440(3) 10.4238(16) 89.966(16) 89.978(13) 89.960(17) V = 1133.6(4) unit cell: 10.4270(6) 10.4270(6) 10.4270(6) 90.0 90.0 90.0 V = 1133.65(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 233 obs out of 251 (total:251,skipped:0) (92.83%) UB - matrix: 0.065956 0.015325 0.006316 ( 0.000018 0.000013 0.000013 ) -0.016309 0.064765 0.013377 ( 0.000023 0.000017 0.000016 ) -0.003130 -0.014554 0.066436 ( 0.000032 0.000023 0.000022 ) M - matrix: 0.004626 0.000000 -0.000010 ( 0.000003 0.000002 0.000002 ) 0.000000 0.004641 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000010 -0.000004 0.004633 ( 0.000002 0.000002 0.000003 ) unit cell: 10.429(3) 10.412(3) 10.421(3) 89.95(2) 89.88(3) 90.00(2) V = 1131.5(6) OTKP changes: 250 1 1 1 OTKP changes: 250 1 1 1 OTKP changes: 250 1 1 1 No constraint UB - matrix: 0.065935 0.015307 0.006300 ( 0.000017 0.000013 0.000013 ) -0.016304 0.064737 0.013387 ( 0.000019 0.000014 0.000014 ) -0.002853 -0.014635 0.066427 ( 0.000017 0.000012 0.000013 ) M - matrix: 0.004621 -0.000004 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000004 0.004639 -0.000009 ( 0.000002 0.000002 0.000001 ) 0.000008 -0.000009 0.004631 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065935 0.015307 0.006300 ( 0.000017 0.000013 0.000013 ) -0.016304 0.064737 0.013387 ( 0.000019 0.000014 0.000014 ) -0.002853 -0.014635 0.066427 ( 0.000017 0.000012 0.000013 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000001 ) UB fit with 250 obs out of 251 (total:251,skipped:0) (99.60%) unit cell: 10.434(3) 10.414(2) 10.422(2) 89.887(16) 90.094(18) 89.945(19) V = 1132.4(4) unit cell: 10.4233(6) 10.4233(6) 10.4233(6) 90.0 90.0 90.0 V = 1132.44(11) Run 5 Omega scan: (-6.000 - 90.000,96 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.183) HKL list info: 1210 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065935 0.015307 0.006300 ( 0.000017 0.000013 0.000013 ) -0.016304 0.064737 0.013387 ( 0.000019 0.000014 0.000014 ) -0.002853 -0.014635 0.066427 ( 0.000017 0.000012 0.000013 ) M - matrix: 0.004621 -0.000004 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000004 0.004639 -0.000009 ( 0.000002 0.000002 0.000001 ) 0.000008 -0.000009 0.004631 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065935 0.015307 0.006300 ( 0.000017 0.000013 0.000013 ) -0.016304 0.064737 0.013387 ( 0.000019 0.000014 0.000014 ) -0.002853 -0.014635 0.066427 ( 0.000017 0.000012 0.000013 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000001 ) UB fit with 250 obs out of 251 (total:251,skipped:0) (99.60%) unit cell: 10.434(3) 10.414(2) 10.422(2) 89.887(16) 90.094(18) 89.945(19) V = 1132.4(4) unit cell: 10.4233(6) 10.4233(6) 10.4233(6) 90.0 90.0 90.0 V = 1132.44(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 250 obs out of 251 (total:251,skipped:0) (99.60%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.067991 -0.000085 0.000071 ( 0.000018 0.000013 0.000013 ) 0.000052 0.068082 -0.000096 ( 0.000015 0.000011 0.000011 ) -0.000015 0.000012 0.068046 ( 0.000017 0.000013 0.000013 ) M - matrix: 0.004623 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004635 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004630 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.067991 -0.000085 0.000071 ( 0.000018 0.000013 0.000013 ) 0.000052 0.068082 -0.000096 ( 0.000015 0.000011 0.000011 ) -0.000015 0.000012 0.068046 ( 0.000017 0.000013 0.000013 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000001 ) UB fit with 250 obs out of 251 (total:251,skipped:0) (99.60%) unit cell: 10.432(3) 10.4183(17) 10.424(2) 89.929(14) 90.047(18) 89.972(17) V = 1132.9(4) unit cell: 10.4248(6) 10.4248(6) 10.4248(6) 90.0 90.0 90.0 V = 1132.93(11) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=96, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=72, end=96, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_72.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_72.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_72.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068103 0.000014 -0.000070 ( 0.000010 0.000010 0.000010 ) -0.000012 0.067995 0.000010 ( 0.000010 0.000011 0.000010 ) 0.000035 -0.000024 0.068094 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004638 0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000000 0.004623 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000001 0.004637 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068103 0.000014 -0.000070 ( 0.000010 0.000010 0.000010 ) -0.000012 0.067995 0.000010 ( 0.000010 0.000011 0.000010 ) 0.000035 -0.000024 0.068094 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 1164 obs out of 1186 (total:1186,skipped:0) (98.15%) unit cell: 10.4151(15) 10.4317(17) 10.4165(12) 89.988(11) 89.971(11) 90.002(12) V = 1131.7(3) unit cell: 10.4211(4) 10.4211(4) 10.4211(4) 90.0 90.0 90.0 V = 1131.72(8) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 103 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof 5095 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:15:23 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.183) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.183) Run 5 Omega scan: (-6.000 - 90.000,96 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.183) PROFFIT INFO: signal sum: min=-775.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-628.3451 max=1278679.6397 PROFFIT INFO: background sum: min=-55.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=383.0000 max=6029.0000 PROFFIT INFO: num of signal pixels: min=41 max=528 PROFFIT INFO: Inet: min=-1005.3522 max=2045887.3750 PROFFIT INFO: sig(Inet): min=52.1952 max=30646.3223 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=218.76 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 421 1691 2600 3129 3382 3933 4284 4491 4822 5040 5095 Percent 8.3 33.2 51.0 61.4 66.4 77.2 84.1 88.1 94.6 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5095 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 5095 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2045887- 132820 509 427094.10 77.97 100.00 132790- 4255 509 31334.38 20.33 100.00 4249- 2205 509 3020.92 7.32 98.62 2203- 1285 509 1677.62 3.98 55.21 1285- 867 509 1055.18 2.40 16.90 866- 574 509 710.09 1.77 8.25 574- 364 509 462.33 1.30 6.09 364- 163 509 262.86 0.77 1.18 163- 23 509 88.03 0.31 0.00 23- -1005 514 -124.74 -0.23 0.00 ------------------------------------------------------------------------------------ 2045887- -1005 5095 46512.27 11.58 38.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 509 113368.10 15.30 68.76 1.73- 1.26 509 91061.08 21.56 61.30 1.26- 1.09 509 63088.69 18.93 66.80 1.09- 0.97 509 56478.91 15.21 36.15 0.97- 0.88 509 16114.80 6.61 43.03 0.88- 0.81 509 54554.70 15.22 38.51 0.81- 0.76 509 19545.18 5.93 18.86 0.76- 0.71 509 21974.47 7.07 17.09 0.71- 0.67 509 25489.75 8.19 28.68 0.67- 0.63 514 3865.89 1.88 7.00 ------------------------------------------------------------------------------------ 6.00- 0.63 5095 46512.27 11.58 38.59 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:15:23 2019 Sorting 5095 observations 53 unique observations with > 7.00 F2/sig(F2) 5095 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 95 508 Total number of frames 508 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 5095 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 9 54 Total number of frames 54 1248 observations > 7.00 F2/sig(F2) 1248 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 9 54 Total number of frames 54 Removing 'redundancy=1' reflections Average redundancy: 18.5 (Out of 1248 removed 6 = 1242, unique = 67) 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 1242 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 9 54 Total number of frames 54 67 unique data precomputed (should be 67) 67 unique data with 1242 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 18.5 (Out of 1242 removed 0 = 1242, unique = 67) 67 unique data precomputed (should be 67) 67 unique data with 1242 observations RMS deviation of equivalent data = 0.28237 Rint = 0.22922 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.22557, wR= 0.30218 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11320, wR= 0.16169, Acormin=0.522, Acormax=1.401, Acor_av=0.980 F test: Probability=1.000, F= 3.954 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09995, wR= 0.14552, Acormin=0.472, Acormax=1.465, Acor_av=0.944 F test: Probability=1.000, F= 1.279 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09980, wR= 0.15185, Acormin=0.545, Acormax=1.494, Acor_av=0.987 F test: Probability=0.000, F= 0.998 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08726, wR= 0.13143, Acormin=0.477, Acormax=1.626, Acor_av=0.955 F test: Probability=1.000, F= 1.302 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07942, wR= 0.12177, Acormin=0.542, Acormax=1.799, Acor_av=0.978 F test: Probability=0.999, F= 1.200 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09819, wR= 0.14645, Acormin=0.443, Acormax=1.573, Acor_av=0.960 F test: Probability=0.000, F= 0.652 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08469, wR= 0.12974, Acormin=0.472, Acormax=1.630, Acor_av=0.942 F test: Probability=0.000, F= 0.875 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07652, wR= 0.11906, Acormin=0.523, Acormax=1.841, Acor_av=0.975 F test: Probability=0.856, F= 1.065 Trying model 9 (ne=6, no=5)... Results: Rint= 0.09804, wR= 0.14024, Acormin=0.155, Acormax=1.072, Acor_av=0.538 F test: Probability=0.000, F= 0.642 Final absorption model (ne=4, no=3): Rint= 0.07942, Acormin=0.542, Acormax=1.799, Acor_av=0.978 Combined refinement in use Rint: 0.23093 There are 54 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: 4, max odd order: 3 (24 parameters) Refinement control: 77 pars with 3003 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.28237 Using Levenberg-Marquardt: 0.00010 New wR= 0.09265 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22922 with corrections 0.06313 Rint for all data: 0.23093 with corrections 0.06587 1 observations identified as outliers and rejected Cycle 2 wR= 0.08599 Using Levenberg-Marquardt: 0.00001 New wR= 0.07811 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22908 with corrections 0.05479 Rint for all data: 0.23093 with corrections 0.06061 0 observations identified as outliers and rejected Cycle 3 wR= 0.07811 Using Levenberg-Marquardt: 0.00000 New wR= 0.07845 Using Levenberg-Marquardt: 0.00001 New wR= 0.07845 Using Levenberg-Marquardt: 0.00010 New wR= 0.07845 Using Levenberg-Marquardt: 0.00100 New wR= 0.07844 Using Levenberg-Marquardt: 0.01000 New wR= 0.07839 Using Levenberg-Marquardt: 0.10000 New wR= 0.07819 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22908 with corrections 0.05438 Rint for all data: 0.23093 with corrections 0.05999 Final wR= 0.07819 Final frame scales: Min= 0.7165 Max= 1.1555 Final absorption correction factors: Amin= 0.3993 Amax= 1.5707 PROFFIT INFO: Inet (after scale3 abspack): min=-1120.9121 max=1379230.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.9158 max=25025.3223 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/104 5095 reflections read from tmp file 219 reflections are rejected (218 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 6 6 2 7 7 9 195 Initial Chi^2= 0.50374 Cycle 1, Chi^2= 1.02396 Current error model SIG(F2)^2 = 63.39*I_RAW + 9.29*I_BACK+(0.03555*)^2 Cycle 2, Chi^2= 1.01534 Current error model SIG(F2)^2 = 76.51*I_RAW + 6.84*I_BACK+(0.02874*)^2 Cycle 3, Chi^2= 1.00698 Current error model SIG(F2)^2 = 81.83*I_RAW + 5.99*I_BACK+(0.02677*)^2 Cycle 4, Chi^2= 1.00240 Current error model SIG(F2)^2 = 83.69*I_RAW + 5.74*I_BACK+(0.02624*)^2 Cycle 5, Chi^2= 1.00072 Current error model SIG(F2)^2 = 84.27*I_RAW + 5.66*I_BACK+(0.02611*)^2 Cycle 6, Chi^2= 1.00020 Current error model SIG(F2)^2 = 84.43*I_RAW + 5.64*I_BACK+(0.02607*)^2 Final Chi^2= 1.00020 Final error model SIG(F2)^2 = 84.43*I_RAW + 5.64*I_BACK+(0.02607*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1379230- 123765 509 403160.79 31.16 100.00 123560- 3662 509 30951.71 13.50 100.00 3657- 2165 509 2835.04 6.40 100.00 2162- 1215 509 1604.54 4.11 71.12 1214- 819 509 1000.66 2.83 29.86 819- 548 509 680.49 2.47 17.09 547- 353 509 445.69 2.04 9.63 352- 161 509 259.46 1.54 4.13 161- 25 509 88.00 0.76 0.00 25- -1121 514 -123.33 -0.50 0.00 ------------------------------------------------------------------------------------ 1379230- -1121 5095 44046.92 6.42 43.14 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 509 108925.33 10.39 72.10 1.73- 1.26 509 86741.95 9.87 65.03 1.26- 1.09 509 59990.90 8.39 71.32 1.09- 0.97 509 52836.52 6.78 38.70 0.97- 0.88 509 13753.40 4.60 51.47 0.88- 0.81 509 53037.02 8.00 46.37 0.81- 0.76 509 18146.45 3.93 22.00 0.76- 0.71 509 20190.69 4.97 22.79 0.71- 0.67 509 23552.35 5.54 33.01 0.67- 0.63 514 3690.98 1.79 8.95 ------------------------------------------------------------------------------------ 6.00- 0.63 5095 44046.92 6.42 43.14 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 509 108925.33 10.39 72.10 6.00- 1.26 1018 97833.64 10.13 68.57 6.00- 1.09 1527 85219.39 9.55 69.48 6.00- 0.97 2036 77123.68 8.86 61.79 6.00- 0.88 2545 64449.62 8.01 59.72 6.00- 0.81 3054 62547.52 8.01 57.50 6.00- 0.76 3563 56204.51 7.42 52.43 6.00- 0.71 4072 51702.78 7.12 48.72 6.00- 0.67 4581 48574.96 6.94 46.98 6.00- 0.63 5095 44046.92 6.42 43.14 ------------------------------------------------------------------------------------ 6.00- 0.63 5095 44046.92 6.42 43.14 Scale applied to data: s=0.725041 (maximum obs:1379230.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.060; Rsigma 0.037: data 5095 -> merged 240 With outlier rejection... Rint 0.051; Rsigma 0.037: data 5071 -> merged 240 Rejected total: 24, method kkm 18, method Blessing 6 Completeness direct cell (a, b, c) = (10.421, 10.421, 10.421), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627276, 6.016620 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.43 - 1.59 21 21 27.90 100.00 586 1.57 - 1.20 21 21 28.95 100.00 608 1.20 - 1.02 21 21 27.19 100.00 571 1.02 - 0.91 21 21 25.90 100.00 544 0.91 - 0.85 21 21 22.86 100.00 480 0.84 - 0.79 21 21 22.48 100.00 472 0.78 - 0.74 21 21 21.43 100.00 450 0.74 - 0.71 21 21 17.71 100.00 372 0.71 - 0.68 21 21 20.10 100.00 422 0.68 - 0.65 23 23 17.00 100.00 391 --------------------------------------------------------------- 10.43 - 0.65 212 212 23.09 100.00 4896 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:15:24 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.415090 10.431684 10.416508 89.9877 89.9712 90.0020 5070 Reflections read from file xs2212a.hkl 5039 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2534 0 3348 3340 5039 N (int>3sigma) = 0 0 0 0 1172 0 1526 1510 2178 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.5 30.0 31.2 Mean int/sigma = 0.0 0.0 0.0 0.0 4.2 0.0 6.5 6.4 6.4 Lattice type: F chosen Volume: 1131.72 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.363 7.367 7.370 60.02 60.03 89.99 Niggli form: a.a = 54.217 b.b = 54.272 c.c = 54.319 b.c = 27.135 a.c = 27.105 a.b = 0.007 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.165 CUBIC F-lattice R(int) = 0.050 [ 4808] Vol = 1131.7 Cell: 10.417 10.415 10.432 90.00 90.01 90.03 Volume: 1131.72 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.120 TETRAGONAL I-lattice R(int) = 0.048 [ 4423] Vol = 565.9 Cell: 7.370 7.371 10.417 90.01 89.97 89.91 Volume: 565.86 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.061 TETRAGONAL I-lattice R(int) = 0.050 [ 4422] Vol = 565.9 Cell: 7.363 7.367 10.432 89.99 89.99 89.99 Volume: 565.86 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.061 ORTHORHOMBIC F-lattice R(int) = 0.048 [ 4370] Vol = 1131.7 Cell: 10.417 10.415 10.432 90.00 90.01 89.97 Volume: 1131.72 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.134 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4350] Vol = 565.9 Cell: 10.417 7.371 7.370 89.91 89.97 90.01 Volume: 565.86 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.008 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4352] Vol = 565.9 Cell: 7.363 7.367 10.432 90.01 90.01 89.99 Volume: 565.86 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.058 MONOCLINIC I-lattice R(int) = 0.046 [ 3826] Vol = 565.9 Cell: 7.370 10.415 7.372 90.02 90.08 90.02 Volume: 565.86 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.056 MONOCLINIC I-lattice R(int) = 0.045 [ 3830] Vol = 565.9 Cell: 7.371 10.417 7.370 90.03 90.09 90.01 Volume: 565.86 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.008 MONOCLINIC I-lattice R(int) = 0.044 [ 3807] Vol = 565.9 Cell: 7.367 7.363 10.432 89.99 90.01 90.01 Volume: 565.86 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.007 MONOCLINIC I-lattice R(int) = 0.045 [ 3822] Vol = 565.9 Cell: 7.363 7.367 10.432 89.99 90.01 90.01 Volume: 565.86 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2779] Vol = 282.9 Cell: 7.363 7.367 7.370 60.02 60.03 89.99 Volume: 282.93 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -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 2534 0 3350 3340 5039 N (int>3sigma) = 0 0 0 0 1172 0 1534 1510 2178 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 30.6 30.0 31.2 Mean int/sigma = 0.0 0.0 0.0 0.0 4.2 0.0 6.4 6.4 6.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.104 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 36 36 373 995 N I>3s 1 1 1 545 0.0 0.0 0.0 1.9 0.8 0.8 0.3 5.2 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 0.050 4463 Fd-3m 1 1 227 C N N N N 37 2284 0.050 4525 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.416508 10.415090 10.431684 90.0020 90.0123 90.0288 ZERR 5.00 0.001226 0.001518 0.001669 0.0124 0.0112 0.0108 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1216889- 135540 506 495 26 19.0 401817.11 31.14 0.046 0.059 114980- 3345 578 573 26 22.0 28297.11 12.66 0.068 0.079 3176- 1502 740 737 26 28.3 2343.91 5.77 0.126 0.182 1440- 895 635 635 26 24.4 1108.98 2.86 0.226 0.296 886- 525 637 637 26 24.5 687.67 2.51 0.282 0.374 519- 319 606 606 26 23.3 402.91 1.78 0.414 0.558 316- 174 496 496 26 19.1 244.73 1.29 0.581 0.865 174- 37 477 476 26 18.3 75.01 0.54 0.889 2.256 35- -356 420 416 32 13.0 -26.94 -0.03 0.970 2.629 ------------------------------------------------------------------------------------------- 1216889- -356 5095 5071 240 21.1 43063.20 6.37 0.051 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-1.45 758 751 26 28.9 119791.98 11.46 0.046 0.056 0.028 1.39-1.09 780 779 26 30.0 45779.96 7.42 0.045 0.057 0.034 1.06-0.94 651 647 26 24.9 40231.42 5.73 0.042 0.053 0.036 0.92-0.85 613 611 26 23.5 44678.70 7.67 0.053 0.069 0.040 0.84-0.78 595 594 26 22.8 26238.26 5.18 0.060 0.083 0.046 0.78-0.73 516 516 26 19.8 9111.69 3.21 0.084 0.100 0.072 0.73-0.69 531 529 27 19.6 19753.67 4.69 0.073 0.088 0.060 0.68-0.66 465 464 27 17.2 15456.09 3.99 0.080 0.108 0.065 0.65-0.63 186 180 30 6.0 8390.14 2.48 0.073 0.076 0.082 ------------------------------------------------------------------------------------------------------ inf-0.63 5095 5071 240 21.1 43063.20 6.37 0.051 0.064 0.037 inf-0.65 4913 4895 211 23.2 44381.14 6.52 0.051 0.064 0.037 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-1.45 751 26 26 100.0 28.9 119791.98 62.59 0.046 0.007 1.39-1.09 779 26 26 100.0 30.0 45779.96 37.51 0.045 0.008 1.06-0.94 647 26 26 100.0 24.9 40231.42 29.44 0.042 0.008 0.92-0.85 611 26 26 100.0 23.5 44678.70 37.12 0.053 0.009 0.84-0.78 594 26 26 100.0 22.8 26238.26 23.87 0.060 0.010 0.78-0.73 516 26 26 100.0 19.8 9111.69 14.56 0.084 0.017 0.73-0.69 529 27 27 100.0 19.6 19753.67 19.73 0.073 0.014 0.68-0.66 464 27 27 100.0 17.2 15456.09 18.25 0.080 0.016 0.65-0.63 180 30 30 100.0 6.0 8390.14 5.97 0.073 0.037 -------------------------------------------------------------------------------------------- inf-0.63 5071 240 240 100.0 21.1 43063.20 31.48 0.051 0.010 inf-0.65 4895 211 211 100.0 23.2 44381.14 32.42 0.051 0.009 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066077 0.014923 0.006907 ( 0.000010 0.000010 0.000010 ) -0.016063 0.064749 0.013208 ( 0.000010 0.000011 0.000011 ) -0.003707 -0.014425 0.066443 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004638 -0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000000 0.004623 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000000 0.004637 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066077 0.014923 0.006907 ( 0.000010 0.000010 0.000010 ) -0.016063 0.064749 0.013208 ( 0.000010 0.000011 0.000011 ) -0.003707 -0.014425 0.066443 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4152(15) 10.4317(17) 10.4165(12) 89.998(11) 89.975(11) 89.994(12) V = 1131.7(3) unit cell: 10.4211(4) 10.4211(4) 10.4211(4) 90.0 90.0 90.0 V = 1131.73(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.183) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.183) Run 5 Omega scan: (-6.000 - 90.000,96 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.183) PROFFIT INFO: signal sum: min=-775.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-628.3451 max=1278679.6397 PROFFIT INFO: background sum: min=-55.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=383.0000 max=6029.0000 PROFFIT INFO: num of signal pixels: min=41 max=528 PROFFIT INFO: Inet: min=-1005.3522 max=2045887.3750 PROFFIT INFO: sig(Inet): min=52.1952 max=30646.3223 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=218.76 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 842 3382 5200 6258 6764 7866 8568 8982 9644 10080 10190 Percent 8.3 33.2 51.0 61.4 66.4 77.2 84.1 88.1 94.6 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5095 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 5095 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2045887- 132820 509 427094.10 77.97 100.00 132790- 4255 509 31334.38 20.33 100.00 4249- 2205 509 3020.92 7.32 98.62 2203- 1285 509 1677.62 3.98 55.21 1285- 867 509 1055.18 2.40 16.90 866- 574 509 710.09 1.77 8.25 574- 364 509 462.33 1.30 6.09 364- 163 509 262.86 0.77 1.18 163- 23 509 88.03 0.31 0.00 23- -1005 514 -124.74 -0.23 0.00 ------------------------------------------------------------------------------------ 2045887- -1005 5095 46512.27 11.58 38.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 509 113368.10 15.30 68.76 1.73- 1.26 509 91061.08 21.56 61.30 1.26- 1.09 509 63088.69 18.93 66.80 1.09- 0.97 509 56478.91 15.21 36.15 0.97- 0.88 509 16114.80 6.61 43.03 0.88- 0.81 509 54554.70 15.22 38.51 0.81- 0.76 509 19545.18 5.93 18.86 0.76- 0.71 509 21974.47 7.07 17.09 0.71- 0.67 509 25489.75 8.19 28.68 0.67- 0.63 514 3865.89 1.88 7.00 ------------------------------------------------------------------------------------ 6.00- 0.63 5095 46512.27 11.58 38.59 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:15:24 2019 Sorting 5095 observations 43 unique observations with > 7.00 F2/sig(F2) 5095 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 95 508 Total number of frames 508 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 12 frame = 1 scale 5095 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 7 44 Total number of frames 44 1248 observations > 7.00 F2/sig(F2) 1248 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 7 44 Total number of frames 44 Removing 'redundancy=1' reflections Average redundancy: 22.7 (Out of 1248 removed 2 = 1246, unique = 55) 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 1246 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 7 44 Total number of frames 44 55 unique data precomputed (should be 55) 55 unique data with 1246 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.7 (Out of 1246 removed 0 = 1246, unique = 55) 55 unique data precomputed (should be 55) 55 unique data with 1246 observations RMS deviation of equivalent data = 0.28267 Rint = 0.22935 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.22570, wR= 0.30247 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11322, wR= 0.16238, Acormin=0.523, Acormax=1.399, Acor_av=0.980 F test: Probability=1.000, F= 3.957 Trying model 2 (ne=2, no=1)... Results: Rint= 0.10001, wR= 0.14622, Acormin=0.471, Acormax=1.464, Acor_av=0.943 F test: Probability=1.000, F= 1.278 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09974, wR= 0.15274, Acormin=0.545, Acormax=1.498, Acor_av=0.988 F test: Probability=0.502, F= 1.000 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08763, wR= 0.13216, Acormin=0.477, Acormax=1.627, Acor_av=0.955 F test: Probability=1.000, F= 1.293 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07985, wR= 0.12267, Acormin=0.539, Acormax=1.800, Acor_av=0.978 F test: Probability=0.999, F= 1.197 Final absorption model (ne=4, no=3): Rint= 0.07985, Acormin=0.539, Acormax=1.800, Acor_av=0.978 Combined refinement in use Rint: 0.23108 There are 44 active scales (one needs to be fixed) Refinement control: frame scale #41 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 67 pars with 2278 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.28267 Using Levenberg-Marquardt: 0.00010 New wR= 0.11008 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22935 with corrections 0.07511 Rint for all data: 0.23108 with corrections 0.07776 5 observations identified as outliers and rejected Cycle 2 wR= 0.09109 Using Levenberg-Marquardt: 0.00001 New wR= 0.07751 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22784 with corrections 0.05713 Rint for all data: 0.23108 with corrections 0.06474 0 observations identified as outliers and rejected Cycle 3 wR= 0.07751 Using Levenberg-Marquardt: 0.00000 New wR= 0.07642 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22784 with corrections 0.05501 Rint for all data: 0.23108 with corrections 0.06234 1 observations identified as outliers and rejected Cycle 4 wR= 0.07272 Using Levenberg-Marquardt: 0.00000 New wR= 0.07196 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22605 with corrections 0.05078 Rint for all data: 0.23108 with corrections 0.05836 0 observations identified as outliers and rejected Cycle 5 wR= 0.07196 Using Levenberg-Marquardt: 0.00000 New wR= 0.07134 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22605 with corrections 0.05084 Rint for all data: 0.23108 with corrections 0.05844 0 observations identified as outliers and rejected Final wR= 0.07134 Final frame scales: Min= 0.7751 Max= 1.2007 Final absorption correction factors: Amin= 0.4017 Amax= 1.5473 PROFFIT INFO: Inet (after scale3 abspack): min=-1153.9413 max=1323625.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=38.6899 max=24711.6387 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/104 5095 reflections read from tmp file 203 reflections are rejected (203 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 2 3 3 3 4 5 3 139 Initial Chi^2= 0.49537 Cycle 1, Chi^2= 1.01955 Current error model SIG(F2)^2 = 61.82*I_RAW + 10.43*I_BACK+(0.03260*)^2 Cycle 2, Chi^2= 1.01577 Current error model SIG(F2)^2 = 75.10*I_RAW + 7.50*I_BACK+(0.02728*)^2 Cycle 3, Chi^2= 1.00540 Current error model SIG(F2)^2 = 79.43*I_RAW + 6.77*I_BACK+(0.02638*)^2 Cycle 4, Chi^2= 1.00135 Current error model SIG(F2)^2 = 80.55*I_RAW + 6.61*I_BACK+(0.02626*)^2 Cycle 5, Chi^2= 1.00032 Current error model SIG(F2)^2 = 80.82*I_RAW + 6.57*I_BACK+(0.02623*)^2 Cycle 6, Chi^2= 1.00007 Current error model SIG(F2)^2 = 80.88*I_RAW + 6.56*I_BACK+(0.02623*)^2 Final Chi^2= 1.00007 Final error model SIG(F2)^2 = 80.88*I_RAW + 6.56*I_BACK+(0.02623*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1323625- 125304 509 402774.03 31.25 100.00 125224- 3633 509 30935.37 13.73 100.00 3624- 2175 509 2837.34 6.50 100.00 2173- 1217 509 1612.14 4.18 72.89 1216- 819 509 1002.64 2.88 32.02 819- 547 509 681.80 2.50 18.27 547- 354 509 445.82 2.04 9.63 354- 161 509 259.44 1.53 4.32 161- 25 509 87.78 0.75 0.20 25- -1154 514 -123.02 -0.50 0.00 ------------------------------------------------------------------------------------ 1323625- -1154 5095 44007.98 6.48 43.69 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 509 108626.80 10.47 72.69 1.73- 1.26 509 86129.92 9.93 65.23 1.26- 1.09 509 60227.22 8.46 72.10 1.09- 0.97 509 52718.14 6.82 38.70 0.97- 0.88 509 13927.88 4.66 52.46 0.88- 0.81 509 53192.06 8.08 46.95 0.81- 0.76 509 18096.23 3.97 22.59 0.76- 0.71 509 20280.59 5.02 23.58 0.71- 0.67 509 23562.65 5.63 33.60 0.67- 0.63 514 3714.15 1.81 9.34 ------------------------------------------------------------------------------------ 6.00- 0.63 5095 44007.98 6.48 43.69 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 509 108626.80 10.47 72.69 6.00- 1.26 1018 97378.36 10.20 68.96 6.00- 1.09 1527 84994.65 9.62 70.01 6.00- 0.97 2036 76925.52 8.92 62.18 6.00- 0.88 2545 64325.99 8.07 60.24 6.00- 0.81 3054 62470.34 8.07 58.02 6.00- 0.76 3563 56131.18 7.48 52.96 6.00- 0.71 4072 51649.86 7.18 49.29 6.00- 0.67 4581 48529.05 7.00 47.54 6.00- 0.63 5095 44007.98 6.48 43.69 ------------------------------------------------------------------------------------ 6.00- 0.63 5095 44007.98 6.48 43.69 Scale applied to data: s=0.755500 (maximum obs:1323625.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.058; Rsigma 0.037: data 5095 -> merged 162 With outlier rejection... Rint 0.052; Rsigma 0.037: data 5079 -> merged 162 Rejected total: 16, method kkm 7, method Blessing 9 Completeness direct cell (a, b, c) = (10.421, 10.421, 10.421), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627278, 6.016641 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.43 - 1.76 14 14 33.36 100.00 467 1.74 - 1.27 14 14 36.93 100.00 517 1.26 - 1.06 14 14 41.29 100.00 578 1.05 - 0.97 14 14 35.79 100.00 501 0.95 - 0.88 14 14 37.21 100.00 521 0.87 - 0.81 14 14 33.29 100.00 466 0.80 - 0.76 14 14 34.43 100.00 482 0.76 - 0.72 14 14 29.29 100.00 410 0.72 - 0.69 14 14 31.86 100.00 446 0.69 - 0.65 19 19 27.00 100.00 513 --------------------------------------------------------------- 10.43 - 0.65 145 145 33.80 100.00 4901 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:15:24 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.415090 10.431684 10.416508 89.9877 89.9712 90.0020 5070 Reflections read from file xs2212a.hkl 5039 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.40 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2534 0 3348 3340 5039 N (int>3sigma) = 0 0 0 0 1172 0 1526 1510 2178 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.5 30.0 31.2 Mean int/sigma = 0.0 0.0 0.0 0.0 4.2 0.0 6.5 6.4 6.4 Lattice type: F chosen Volume: 1131.72 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.363 7.367 7.370 60.02 60.03 89.99 Niggli form: a.a = 54.217 b.b = 54.272 c.c = 54.319 b.c = 27.135 a.c = 27.105 a.b = 0.007 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.165 CUBIC F-lattice R(int) = 0.050 [ 4808] Vol = 1131.7 Cell: 10.417 10.415 10.432 90.00 90.01 90.03 Volume: 1131.72 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.120 TETRAGONAL I-lattice R(int) = 0.048 [ 4423] Vol = 565.9 Cell: 7.370 7.371 10.417 90.01 89.97 89.91 Volume: 565.86 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.061 TETRAGONAL I-lattice R(int) = 0.050 [ 4422] Vol = 565.9 Cell: 7.363 7.367 10.432 89.99 89.99 89.99 Volume: 565.86 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.061 ORTHORHOMBIC F-lattice R(int) = 0.048 [ 4370] Vol = 1131.7 Cell: 10.417 10.415 10.432 90.00 90.01 89.97 Volume: 1131.72 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.134 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4350] Vol = 565.9 Cell: 10.417 7.371 7.370 89.91 89.97 90.01 Volume: 565.86 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.008 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4352] Vol = 565.9 Cell: 7.363 7.367 10.432 90.01 90.01 89.99 Volume: 565.86 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.058 MONOCLINIC I-lattice R(int) = 0.046 [ 3826] Vol = 565.9 Cell: 7.370 10.415 7.372 90.02 90.08 90.02 Volume: 565.86 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.056 MONOCLINIC I-lattice R(int) = 0.045 [ 3830] Vol = 565.9 Cell: 7.371 10.417 7.370 90.03 90.09 90.01 Volume: 565.86 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.008 MONOCLINIC I-lattice R(int) = 0.044 [ 3807] Vol = 565.9 Cell: 7.367 7.363 10.432 89.99 90.01 90.01 Volume: 565.86 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.007 MONOCLINIC I-lattice R(int) = 0.045 [ 3822] Vol = 565.9 Cell: 7.363 7.367 10.432 89.99 90.01 90.01 Volume: 565.86 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2779] Vol = 282.9 Cell: 7.363 7.367 7.370 60.02 60.03 89.99 Volume: 282.93 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -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 2534 0 3350 3340 5039 N (int>3sigma) = 0 0 0 0 1172 0 1534 1510 2178 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 30.6 30.0 31.2 Mean int/sigma = 0.0 0.0 0.0 0.0 4.2 0.0 6.4 6.4 6.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.104 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 36 36 373 995 N I>3s 1 1 1 545 0.0 0.0 0.0 1.9 0.8 0.8 0.3 5.2 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 0.050 4463 Fd-3m 1 1 227 C N N N N 37 2284 0.050 4525 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.416508 10.415090 10.431684 90.0020 90.0123 90.0288 ZERR 5.00 0.001226 0.001518 0.001669 0.0124 0.0112 0.0108 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1217356- 95698 619 609 27 22.6 349505.24 29.48 0.048 0.059 81306- 1919 967 965 27 35.7 5620.76 8.74 0.086 0.098 1787- 826 1019 1017 27 37.7 1192.62 3.10 0.214 0.287 812- 345 1001 1000 27 37.0 527.11 2.17 0.343 0.482 343- 69 753 752 27 27.9 227.54 1.18 0.598 0.963 64- -154 736 736 27 27.3 10.37 0.20 0.960 3.625 ------------------------------------------------------------------------------------------- 1217356- -154 5095 5079 162 31.4 43353.31 6.45 0.052 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-1.27 987 982 27 36.4 97595.85 10.36 0.046 0.054 0.029 1.26-0.97 1083 1079 28 38.5 52832.22 7.24 0.047 0.060 0.034 0.95-0.81 989 987 28 35.3 34526.55 6.52 0.055 0.070 0.042 0.80-0.73 872 871 27 32.3 18785.12 4.42 0.059 0.077 0.053 0.72-0.67 775 774 27 28.7 19509.85 4.80 0.078 0.102 0.060 0.66-0.63 389 386 25 15.4 4679.30 1.99 0.102 0.077 0.113 ------------------------------------------------------------------------------------------------------ inf-0.63 5095 5079 162 31.4 43353.31 6.45 0.052 0.062 0.037 inf-0.65 4913 4899 144 34.0 44682.62 6.60 0.051 0.062 0.036 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-1.27 982 27 27 100.0 36.4 97595.85 60.64 0.046 0.007 1.26-0.97 1079 28 28 100.0 38.5 52832.22 42.57 0.047 0.007 0.95-0.81 987 28 28 100.0 35.3 34526.55 39.08 0.055 0.009 0.80-0.73 871 27 27 100.0 32.3 18785.12 22.98 0.059 0.011 0.72-0.67 774 27 27 100.0 28.7 19509.85 27.57 0.078 0.012 0.66-0.63 386 25 25 100.0 15.4 4679.30 7.95 0.102 0.031 -------------------------------------------------------------------------------------------- inf-0.63 5079 162 162 100.0 31.4 43353.31 37.11 0.052 0.009 inf-0.65 4899 144 144 100.0 34.0 44682.62 38.24 0.051 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:16:26 2019) ID: 3668; threads 39; handles 810; mem 515832.00 (1196500.00)kB; time: 1w 5d 0h 27m 14s MEMORY INFO: Memory PF:226.0, Ph:557.0, V:1168.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:503.7,peak PF: 700.2, WS: 471.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:229.0, Ph:558.0, V:1170.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:505.5,peak PF: 700.2, WS: 473.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:16:26 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000013 0.000014 0.000014 ) -0.003867 -0.014380 0.066544 ( 0.000015 0.000017 0.000016 ) 10.42433 ( 0.00235 ) 10.43788 ( 0.00221 ) 10.40727 ( 0.00244 ) 89.88512 ( 0.01820 ) 89.79539 ( 0.01871 ) 90.20497 ( 0.01805 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:16:27 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000013 0.000014 0.000014 ) -0.003867 -0.014380 0.066544 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004633 0.000003 -0.000008 ( 0.000002 0.000001 0.000002 ) 0.000003 0.004618 -0.000005 ( 0.000001 0.000002 0.000001 ) -0.000008 -0.000005 0.004648 ( 0.000002 0.000001 0.000002 ) unit cell: 10.424(2) 10.438(2) 10.407(2) 89.885(18) 89.795(19) 90.205(18) V = 1132.4(4) unit cell: 10.4207(8) 10.4207(8) 10.4207(8) 90.0 90.0 90.0 V = 1131.60(15) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.938 ( 0.170) | 0.923 ( 0.398) | 1.01- 0.88 | 22 | 0.957 ( 0.073) | 1.004 ( 0.124) | 1.180 ( 0.493) | 0.88- 0.79 | 22 | 0.985 ( 0.059) | 1.028 ( 0.140) | 1.234 ( 0.387) | 0.79- 0.70 | 22 | 0.984 ( 0.041) | 0.962 ( 0.107) | 1.276 ( 0.475) | 0.70- 0.63 | 22 | 0.943 ( 0.038) | 0.917 ( 0.081) | 1.311 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 220 | 0.933 ( 0.193) | 0.943 ( 0.158) | 1.113 ( 0.914) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.87 | 25 | 0.945 ( 0.067) | 0.936 ( 0.094) | 1.074 ( 0.403) | 0.86- 0.73 | 25 | 0.958 ( 0.050) | 0.919 ( 0.091) | 1.335 ( 0.450) | 0.73- 0.63 | 29 | 0.929 ( 0.037) | 0.880 ( 0.095) | 1.340 ( 0.463) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 254 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.061 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_5_78.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_78.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_5_78.rpb PROFFITPEAK info: 548 peaks in the peak location table UB fit with 236 obs out of 294 (total:295,skipped:1) (80.27%) UB - matrix: 0.066015 0.015272 0.006427 ( 0.000038 0.000030 0.000026 ) -0.016260 0.064753 0.013274 ( 0.000038 0.000030 0.000025 ) -0.003266 -0.014514 0.066428 ( 0.000042 0.000033 0.000028 ) M - matrix: 0.004633 0.000003 -0.000008 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004637 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000008 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.421(6) 10.416(5) 10.424(4) 89.92(4) 89.90(4) 90.03(4) V = 1131.5(9) UB fit with 236 obs out of 294 (total:295,skipped:1) (80.27%) UB - matrix: 0.066015 0.015272 0.006427 ( 0.000038 0.000030 0.000026 ) -0.016260 0.064753 0.013274 ( 0.000038 0.000030 0.000025 ) -0.003266 -0.014514 0.066428 ( 0.000042 0.000033 0.000028 ) M - matrix: 0.004633 0.000003 -0.000008 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004637 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000008 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.421(6) 10.416(5) 10.424(4) 89.92(4) 89.90(4) 90.03(4) V = 1131.5(9) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 No constraint UB - matrix: 0.066000 0.015410 0.006314 ( 0.000032 0.000025 0.000024 ) -0.016349 0.064723 0.013346 ( 0.000031 0.000024 0.000023 ) -0.002934 -0.014609 0.066406 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000002 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000002 0.004640 -0.000009 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000009 0.004628 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066000 0.015410 0.006314 ( 0.000032 0.000025 0.000024 ) -0.016349 0.064723 0.013346 ( 0.000031 0.000024 0.000023 ) -0.002934 -0.014609 0.066406 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 268 obs out of 294 (total:295,skipped:1) (91.16%) unit cell: 10.422(5) 10.413(4) 10.427(3) 89.89(3) 90.05(3) 90.02(3) V = 1131.5(7) unit cell: 10.4205(10) 10.4205(10) 10.4205(10) 90.0 90.0 90.0 V = 1131.54(19) UB fit with 268 obs out of 294 (total:295,skipped:1) (91.16%) UB - matrix: 0.066000 0.015410 0.006314 ( 0.000032 0.000025 0.000024 ) -0.016349 0.064723 0.013346 ( 0.000031 0.000024 0.000023 ) -0.002934 -0.014609 0.066406 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000002 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000002 0.004640 -0.000009 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000009 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.413(4) 10.427(3) 89.89(3) 90.05(3) 90.02(3) V = 1131.5(7) 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 1 295 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Run 5 Omega scan: (-6.000 - 96.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066000 0.015410 0.006314 ( 0.000032 0.000025 0.000024 ) -0.016349 0.064723 0.013346 ( 0.000031 0.000024 0.000023 ) -0.002934 -0.014609 0.066406 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000002 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000002 0.004640 -0.000009 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000009 0.004628 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066000 0.015410 0.006314 ( 0.000032 0.000025 0.000024 ) -0.016349 0.064723 0.013346 ( 0.000031 0.000024 0.000023 ) -0.002934 -0.014609 0.066406 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 268 obs out of 294 (total:295,skipped:1) (91.16%) unit cell: 10.422(5) 10.413(4) 10.427(3) 89.89(3) 90.05(3) 90.02(3) V = 1131.5(7) unit cell: 10.4205(10) 10.4205(10) 10.4205(10) 90.0 90.0 90.0 V = 1131.54(19) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 269 obs out of 294 (total:295,skipped:1) (91.50%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_78.rpb 0 of 273 peaks identified as outliers and rejected 273 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 273 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 273 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 27 | 0.891 ( 0.103) | 0.900 ( 0.132) | 0.820 ( 0.201) | 2.13- 1.75 | 27 | 0.909 ( 0.127) | 0.998 ( 0.364) | 0.964 ( 0.572) | 1.75- 1.56 | 27 | 0.956 ( 0.114) | 0.968 ( 0.145) | 0.966 ( 0.413) | 1.56- 1.35 | 27 | 0.956 ( 0.098) | 0.967 ( 0.158) | 0.788 ( 0.304) | 1.35- 1.19 | 27 | 0.934 ( 0.096) | 0.966 ( 0.153) | 0.706 ( 0.264) | 1.19- 1.09 | 27 | 0.992 ( 0.061) | 1.026 ( 0.114) | 0.860 ( 0.277) | 1.09- 0.97 | 27 | 1.000 ( 0.081) | 1.059 ( 0.115) | 0.955 ( 0.415) | 0.94- 0.87 | 27 | 1.000 ( 0.065) | 0.988 ( 0.123) | 1.079 ( 0.275) | 0.87- 0.73 | 27 | 1.044 ( 0.051) | 1.039 ( 0.136) | 1.159 ( 0.453) | 0.73- 0.63 | 30 | 1.008 ( 0.040) | 1.008 ( 0.118) | 1.088 ( 0.374) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 273 | 0.969 ( 0.099) | 0.992 ( 0.176) | 0.940 ( 0.395) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 272 obs out of 273 (total:273,skipped:0) (99.63%) UB - matrix: 0.066031 0.015428 0.006411 ( 0.000019 0.000014 0.000015 ) -0.016409 0.064852 0.013485 ( 0.000023 0.000017 0.000018 ) -0.002786 -0.014650 0.066451 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004637 -0.000005 0.000017 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004658 -0.000000 ( 0.000002 0.000002 0.000002 ) 0.000017 -0.000000 0.004639 ( 0.000002 0.000002 0.000002 ) unit cell: 10.416(3) 10.392(3) 10.414(2) 90.000(19) 90.21(2) 89.94(2) V = 1127.3(5) OTKP changes: 272 1 1 1 OTKP changes: 272 1 1 1 OTKP changes: 272 1 1 1 No constraint UB - matrix: 0.065961 0.015330 0.006302 ( 0.000017 0.000012 0.000013 ) -0.016321 0.064754 0.013401 ( 0.000019 0.000014 0.000015 ) -0.002848 -0.014646 0.066460 ( 0.000016 0.000012 0.000013 ) M - matrix: 0.004625 -0.000004 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000002 0.000002 0.000001 ) 0.000008 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065961 0.015330 0.006302 ( 0.000017 0.000012 0.000013 ) -0.016321 0.064754 0.013401 ( 0.000019 0.000014 0.000015 ) -0.002848 -0.014646 0.066460 ( 0.000016 0.000012 0.000013 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 272 obs out of 273 (total:273,skipped:0) (99.63%) unit cell: 10.429(2) 10.410(2) 10.4171(19) 89.889(16) 90.095(17) 89.951(19) V = 1131.0(4) unit cell: 10.4188(6) 10.4188(6) 10.4188(6) 90.0 90.0 90.0 V = 1130.99(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 96.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065961 0.015330 0.006302 ( 0.000017 0.000012 0.000013 ) -0.016321 0.064754 0.013401 ( 0.000019 0.000014 0.000015 ) -0.002848 -0.014646 0.066460 ( 0.000016 0.000012 0.000013 ) M - matrix: 0.004625 -0.000004 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000002 0.000002 0.000001 ) 0.000008 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065961 0.015330 0.006302 ( 0.000017 0.000012 0.000013 ) -0.016321 0.064754 0.013401 ( 0.000019 0.000014 0.000015 ) -0.002848 -0.014646 0.066460 ( 0.000016 0.000012 0.000013 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 272 obs out of 273 (total:273,skipped:0) (99.63%) unit cell: 10.429(2) 10.410(2) 10.4171(19) 89.889(16) 90.095(17) 89.951(19) V = 1131.0(4) unit cell: 10.4188(6) 10.4188(6) 10.4188(6) 90.0 90.0 90.0 V = 1130.99(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 272 obs out of 273 (total:273,skipped:0) (99.63%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_78.rpb 0 of 267 peaks identified as outliers and rejected 267 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 267 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 267 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.892 ( 0.100) | 0.908 ( 0.135) | 0.792 ( 0.163) | 2.12- 1.75 | 27 | 0.929 ( 0.129) | 1.037 ( 0.460) | 0.969 ( 0.469) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.006 ( 0.144) | 0.998 ( 0.441) | 1.46- 1.35 | 27 | 0.946 ( 0.092) | 0.959 ( 0.160) | 0.748 ( 0.295) | 1.30- 1.16 | 27 | 0.949 ( 0.102) | 0.980 ( 0.153) | 0.750 ( 0.283) | 1.16- 1.06 | 27 | 0.995 ( 0.070) | 1.044 ( 0.106) | 0.915 ( 0.336) | 1.06- 0.89 | 27 | 0.995 ( 0.071) | 1.042 ( 0.123) | 0.995 ( 0.360) | 0.89- 0.86 | 27 | 1.008 ( 0.063) | 1.006 ( 0.113) | 1.123 ( 0.416) | 0.86- 0.72 | 27 | 1.045 ( 0.045) | 1.021 ( 0.132) | 1.167 ( 0.444) | 0.72- 0.63 | 24 | 1.004 ( 0.043) | 1.026 ( 0.126) | 1.059 ( 0.355) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 267 | 0.974 ( 0.097) | 1.003 ( 0.198) | 0.950 ( 0.394) | 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- 9.9 | 120 | 0.987 ( 0.040) | 1.031 ( 0.067) | 1.107 ( 0.469) | 10.0-14.6 | 120 | 0.994 ( 0.046) | 1.049 ( 0.069) | 1.118 ( 0.543) | 14.6-18.7 | 120 | 0.995 ( 0.194) | 1.033 ( 0.101) | 1.142 ( 1.017) | 18.8-23.4 | 120 | 0.970 ( 0.059) | 1.014 ( 0.083) | 0.918 ( 0.417) | 23.4-26.8 | 120 | 0.970 ( 0.062) | 1.001 ( 0.095) | 0.999 ( 0.439) | 26.9-32.0 | 120 | 0.944 ( 0.079) | 0.963 ( 0.106) | 0.943 ( 0.448) | 32.0-36.2 | 120 | 0.927 ( 0.157) | 0.926 ( 0.142) | 1.040 ( 0.666) | 36.2-38.9 | 120 | 0.882 ( 0.103) | 0.876 ( 0.258) | 1.027 ( 0.478) | 38.9-41.9 | 120 | 0.908 ( 0.094) | 0.859 ( 0.129) | 1.030 ( 0.474) | 41.9-50.1 | 122 | 0.863 ( 0.123) | 0.796 ( 0.143) | 0.928 ( 0.444) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1202 | 0.944 ( 0.116) | 0.955 ( 0.154) | 1.025 ( 0.571) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.14 e2 dimension: a=-0.0067 b=1.23 e3 dimension: a=0.0006 b=1.09 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 4497 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563271 PROFFITPEAK - Finished at Wed Aug 21 14:16:44 2019 PROFFITMAIN - Started at Wed Aug 21 14:16:44 2019 OTKP changes: 954 2 4 5 OTKP changes: 954 2 4 5 OTKP changes: 954 2 4 5 No constraint UB - matrix: 0.066034 0.015003 0.006775 ( 0.000014 0.000016 0.000015 ) -0.016041 0.064686 0.013093 ( 0.000013 0.000015 0.000015 ) -0.003774 -0.014361 0.066570 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004632 0.000007 -0.000014 ( 0.000002 0.000001 0.000001 ) 0.000007 0.004616 -0.000007 ( 0.000001 0.000002 0.000002 ) -0.000014 -0.000007 0.004649 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: 0.066034 0.015003 0.006775 ( 0.000014 0.000016 0.000015 ) -0.016041 0.064686 0.013093 ( 0.000013 0.000015 0.000015 ) -0.003774 -0.014361 0.066570 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000001 ) UB fit with 965 obs out of 1202 (total:1202,skipped:0) (80.28%) unit cell: 10.422(2) 10.440(2) 10.403(2) 89.908(19) 89.828(18) 90.089(18) V = 1131.9(4) unit cell: 10.4217(8) 10.4217(8) 10.4217(8) 90.0 90.0 90.0 V = 1131.93(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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 187 obs out of 220 (total:220,skipped:0) (85.00%) UB - matrix: 0.066500 0.011702 0.008960 ( 0.000032 0.000043 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000030 0.000040 0.000034 ) -0.006052 -0.013931 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.60(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004603 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 220 (total:220,skipped:0) (85.91%) unit cell: 10.406(5) 10.502(6) 10.456(6) 90.61(5) 90.19(4) 89.64(4) V = 1143(1) unit cell: 10.4543(19) 10.4543(19) 10.4543(19) 90.0 90.0 90.0 V = 1142.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 220 (total:220,skipped:0) (92.27%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004644 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 220 (total:220,skipped:0) (93.64%) unit cell: 10.409(4) 10.492(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1140.0(9) unit cell: 10.4466(13) 10.4466(13) 10.4466(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.066336 0.014186 0.006779 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064704 0.012861 ( 0.000017 0.000022 0.000023 ) -0.004076 -0.014197 0.066901 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.393(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4047(5) 10.4047(5) 10.4047(5) 90.0 90.0 90.0 V = 1126.40(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065852 0.015174 0.006784 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064731 0.013265 ( 0.000016 0.000011 0.000016 ) -0.003662 -0.014496 0.066467 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004608 0.000012 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000012 0.004630 -0.000002 ( 0.000001 0.000002 0.000001 ) -0.000010 -0.000002 0.004640 ( 0.000002 0.000001 0.000003 ) unit cell: 10.449(3) 10.4237(19) 10.413(3) 89.977(18) 89.88(2) 90.150(18) V = 1134.1(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065825 0.015156 0.006802 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064736 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003669 -0.014466 0.066447 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004604 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 0.000000 0.004637 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065825 0.015156 0.006802 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064736 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003669 -0.014466 0.066447 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.453(3) 10.4244(19) 10.416(3) 90.001(18) 89.89(2) 90.140(18) V = 1135.0(5) unit cell: 10.4312(6) 10.4312(6) 10.4312(6) 90.0 90.0 90.0 V = 1135.03(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.174) HKL list info: 1274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065825 0.015156 0.006802 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064736 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003669 -0.014466 0.066447 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004604 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 0.000000 0.004637 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065825 0.015156 0.006802 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064736 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003669 -0.014466 0.066447 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.453(3) 10.4244(19) 10.416(3) 90.001(18) 89.89(2) 90.140(18) V = 1135.0(5) unit cell: 10.4312(6) 10.4312(6) 10.4312(6) 90.0 90.0 90.0 V = 1135.03(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065825 0.015156 0.006802 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064736 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003669 -0.014466 0.066447 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004604 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 0.000000 0.004637 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065825 0.015156 0.006802 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064736 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003669 -0.014466 0.066447 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.453(3) 10.4244(19) 10.416(3) 90.001(18) 89.89(2) 90.140(18) V = 1135.0(5) unit cell: 10.4312(6) 10.4312(6) 10.4312(6) 90.0 90.0 90.0 V = 1135.03(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066075 0.015219 0.006573 ( 0.000014 0.000018 0.000015 ) -0.016357 0.064708 0.012945 ( 0.000012 0.000016 0.000014 ) -0.003384 -0.014182 0.066473 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004645 -0.000005 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004620 -0.000005 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000005 0.004629 ( 0.000001 0.000001 0.000002 ) unit cell: 10.407(2) 10.436(2) 10.4248(18) 89.937(16) 89.971(16) 89.941(18) V = 1132.2(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066045 0.015195 0.006551 ( 0.000013 0.000018 0.000015 ) -0.016307 0.064679 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003373 -0.014171 0.066486 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004639 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004615 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004631 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066045 0.015195 0.006551 ( 0.000013 0.000018 0.000015 ) -0.016307 0.064679 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003373 -0.014171 0.066486 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.414(2) 10.441(2) 10.4227(18) 89.948(16) 89.964(16) 89.958(18) V = 1133.3(4) unit cell: 10.4258(5) 10.4258(5) 10.4258(5) 90.0 90.0 90.0 V = 1133.26(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.174) HKL list info: 1300 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066045 0.015195 0.006551 ( 0.000013 0.000018 0.000015 ) -0.016307 0.064679 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003373 -0.014171 0.066486 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004639 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004615 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004631 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066045 0.015195 0.006551 ( 0.000013 0.000018 0.000015 ) -0.016307 0.064679 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003373 -0.014171 0.066486 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.414(2) 10.441(2) 10.4227(18) 89.948(16) 89.964(16) 89.958(18) V = 1133.3(4) unit cell: 10.4258(5) 10.4258(5) 10.4258(5) 90.0 90.0 90.0 V = 1133.26(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068097 -0.000048 -0.000033 ( 0.000011 0.000015 0.000012 ) 0.000002 0.067949 -0.000048 ( 0.000013 0.000018 0.000015 ) 0.000006 0.000008 0.068054 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004637 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004617 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004631 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068097 -0.000048 -0.000033 ( 0.000011 0.000015 0.000012 ) 0.000002 0.067949 -0.000048 ( 0.000013 0.000018 0.000015 ) 0.000006 0.000008 0.068054 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.4160(17) 10.439(3) 10.4226(16) 89.966(16) 89.978(13) 89.961(17) V = 1133.3(4) unit cell: 10.4258(5) 10.4258(5) 10.4258(5) 90.0 90.0 90.0 V = 1133.25(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 246 obs out of 267 (total:267,skipped:0) (92.13%) UB - matrix: 0.065947 0.015333 0.006314 ( 0.000017 0.000013 0.000013 ) -0.016303 0.064759 0.013384 ( 0.000022 0.000017 0.000017 ) -0.003174 -0.014530 0.066439 ( 0.000032 0.000025 0.000025 ) M - matrix: 0.004625 0.000002 -0.000013 ( 0.000002 0.000002 0.000002 ) 0.000002 0.004640 -0.000002 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000002 0.004633 ( 0.000002 0.000002 0.000003 ) unit cell: 10.430(3) 10.413(3) 10.421(4) 89.98(3) 89.84(3) 90.02(2) V = 1131.7(6) OTKP changes: 266 1 1 1 OTKP changes: 266 1 1 1 OTKP changes: 266 1 1 1 No constraint UB - matrix: 0.065943 0.015328 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016325 0.064731 0.013400 ( 0.000018 0.000014 0.000014 ) -0.002846 -0.014641 0.066437 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004623 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004639 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065943 0.015328 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016325 0.064731 0.013400 ( 0.000018 0.000014 0.000014 ) -0.002846 -0.014641 0.066437 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 266 obs out of 267 (total:267,skipped:0) (99.63%) unit cell: 10.432(2) 10.414(2) 10.4206(19) 89.891(16) 90.090(17) 89.948(18) V = 1132.0(4) unit cell: 10.4220(6) 10.4220(6) 10.4220(6) 90.0 90.0 90.0 V = 1132.03(11) Run 5 Omega scan: (-6.000 - 96.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.174) HKL list info: 1276 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065943 0.015328 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016325 0.064731 0.013400 ( 0.000018 0.000014 0.000014 ) -0.002846 -0.014641 0.066437 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004623 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004639 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065943 0.015328 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016325 0.064731 0.013400 ( 0.000018 0.000014 0.000014 ) -0.002846 -0.014641 0.066437 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 266 obs out of 267 (total:267,skipped:0) (99.63%) unit cell: 10.432(2) 10.414(2) 10.4206(19) 89.891(16) 90.090(17) 89.948(18) V = 1132.0(4) unit cell: 10.4220(6) 10.4220(6) 10.4220(6) 90.0 90.0 90.0 V = 1132.03(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 266 obs out of 267 (total:267,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068005 -0.000087 0.000068 ( 0.000017 0.000013 0.000013 ) 0.000055 0.068081 -0.000085 ( 0.000014 0.000010 0.000011 ) -0.000016 0.000010 0.068056 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004625 -0.000002 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004635 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000003 -0.000005 0.004632 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068005 -0.000087 0.000068 ( 0.000017 0.000013 0.000013 ) 0.000055 0.068081 -0.000085 ( 0.000014 0.000010 0.000011 ) -0.000016 0.000010 0.068056 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 266 obs out of 267 (total:267,skipped:0) (99.63%) unit cell: 10.430(3) 10.4185(16) 10.4223(19) 89.937(14) 90.043(17) 89.973(16) V = 1132.6(4) unit cell: 10.4236(6) 10.4236(6) 10.4236(6) 90.0 90.0 90.0 V = 1132.55(11) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_78.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068104 0.000014 -0.000068 ( 0.000010 0.000010 0.000010 ) -0.000012 0.067999 0.000015 ( 0.000010 0.000011 0.000010 ) 0.000034 -0.000023 0.068100 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004638 0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000000 0.004624 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000001 0.004638 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068104 0.000014 -0.000068 ( 0.000010 0.000010 0.000010 ) -0.000012 0.067999 0.000015 ( 0.000010 0.000011 0.000010 ) 0.000034 -0.000023 0.068100 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000000 ) UB fit with 1181 obs out of 1202 (total:1202,skipped:0) (98.25%) unit cell: 10.4150(15) 10.4311(17) 10.4156(12) 89.993(11) 89.971(11) 90.002(12) V = 1131.6(3) unit cell: 10.4206(4) 10.4206(4) 10.4206(4) 90.0 90.0 90.0 V = 1131.55(7) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 104 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof 5159 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:16:52 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.174) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.174) Run 5 Omega scan: (-6.000 - 96.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.174) PROFFIT INFO: signal sum: min=-775.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-679.7787 max=1265214.6783 PROFFIT INFO: background sum: min=-55.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=383.0000 max=6324.0000 PROFFIT INFO: num of signal pixels: min=41 max=555 PROFFIT INFO: Inet: min=-1087.6460 max=2024343.3750 PROFFIT INFO: sig(Inet): min=52.2346 max=30600.2930 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=218.80 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 429 1712 2630 3170 3421 3981 4338 4545 4879 5102 5159 Percent 8.3 33.2 51.0 61.4 66.3 77.2 84.1 88.1 94.6 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5159 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 5159 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2024343- 133510 515 434984.49 78.40 100.00 133403- 4275 515 32058.14 20.44 100.00 4270- 2219 515 3031.49 7.36 98.25 2209- 1298 515 1687.46 3.99 54.56 1297- 873 515 1063.65 2.44 18.06 871- 576 515 713.40 1.77 7.96 575- 365 515 463.97 1.30 6.02 364- 168 515 266.20 0.78 1.36 168- 25 515 90.17 0.31 0.00 25- -1088 524 -122.43 -0.23 0.00 ------------------------------------------------------------------------------------ 2024343- -1088 5159 47340.71 11.64 38.55 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 515 117843.92 15.44 68.74 1.73- 1.26 515 92389.65 21.50 61.36 1.26- 1.09 515 63808.22 19.07 66.80 1.09- 0.97 515 57940.03 15.55 36.50 0.97- 0.88 515 12984.33 5.85 42.14 0.88- 0.81 515 58412.36 16.09 39.42 0.81- 0.76 515 19312.89 5.85 18.25 0.76- 0.71 515 21739.70 7.02 17.28 0.71- 0.67 515 25938.37 8.31 29.13 0.67- 0.63 524 3798.57 1.85 6.49 ------------------------------------------------------------------------------------ 6.00- 0.63 5159 47340.71 11.64 38.55 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:16:52 2019 Sorting 5159 observations 53 unique observations with > 7.00 F2/sig(F2) 5159 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 101 514 Total number of frames 514 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 5159 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 10 55 Total number of frames 55 1267 observations > 7.00 F2/sig(F2) 1267 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 10 55 Total number of frames 55 Removing 'redundancy=1' reflections Average redundancy: 18.8 (Out of 1267 removed 7 = 1260, unique = 67) 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 1260 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 10 55 Total number of frames 55 67 unique data precomputed (should be 67) 67 unique data with 1260 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 18.8 (Out of 1260 removed 0 = 1260, unique = 67) 67 unique data precomputed (should be 67) 67 unique data with 1260 observations RMS deviation of equivalent data = 0.28611 Rint = 0.23433 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.23091, wR= 0.30876 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11180, wR= 0.16118, Acormin=0.514, Acormax=1.404, Acor_av=0.976 F test: Probability=1.000, F= 4.248 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09942, wR= 0.14538, Acormin=0.470, Acormax=1.465, Acor_av=0.939 F test: Probability=1.000, F= 1.261 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09853, wR= 0.15129, Acormin=0.533, Acormax=1.497, Acor_av=0.983 F test: Probability=0.589, F= 1.013 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08708, wR= 0.13154, Acormin=0.474, Acormax=1.624, Acor_av=0.950 F test: Probability=1.000, F= 1.294 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07891, wR= 0.12181, Acormin=0.537, Acormax=1.798, Acor_av=0.973 F test: Probability=0.999, F= 1.210 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09785, wR= 0.14584, Acormin=0.442, Acormax=1.575, Acor_av=0.956 F test: Probability=0.000, F= 0.649 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08461, wR= 0.12967, Acormin=0.470, Acormax=1.632, Acor_av=0.938 F test: Probability=0.000, F= 0.865 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07634, wR= 0.11916, Acormin=0.520, Acormax=1.839, Acor_av=0.969 F test: Probability=0.825, F= 1.057 Trying model 9 (ne=6, no=5)... Results: Rint= 0.09806, wR= 0.13891, Acormin=0.172, Acormax=1.085, Acor_av=0.545 F test: Probability=0.000, F= 0.634 Final absorption model (ne=4, no=3): Rint= 0.07891, Acormin=0.537, Acormax=1.798, Acor_av=0.973 Combined refinement in use Rint: 0.23596 There are 55 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: 4, max odd order: 3 (24 parameters) Refinement control: 78 pars with 3081 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.28611 Using Levenberg-Marquardt: 0.00010 New wR= 0.09156 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23433 with corrections 0.06201 Rint for all data: 0.23596 with corrections 0.06471 1 observations identified as outliers and rejected Cycle 2 wR= 0.08530 Using Levenberg-Marquardt: 0.00001 New wR= 0.07840 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23414 with corrections 0.05523 Rint for all data: 0.23596 with corrections 0.06089 2 observations identified as outliers and rejected Cycle 3 wR= 0.07282 Using Levenberg-Marquardt: 0.00000 New wR= 0.07520 Using Levenberg-Marquardt: 0.00001 New wR= 0.07520 Using Levenberg-Marquardt: 0.00010 New wR= 0.07520 Using Levenberg-Marquardt: 0.00100 New wR= 0.07516 Using Levenberg-Marquardt: 0.01000 New wR= 0.07484 Using Levenberg-Marquardt: 0.10000 New wR= 0.07352 Using Levenberg-Marquardt: 1.00000 New wR= 0.07259 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23325 with corrections 0.05320 Rint for all data: 0.23596 with corrections 0.05956 0 observations identified as outliers and rejected Cycle 4 wR= 0.07259 Using Levenberg-Marquardt: 0.10000 New wR= 0.07336 Using Levenberg-Marquardt: 1.00000 New wR= 0.07265 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23325 with corrections 0.05282 Rint for all data: 0.23596 with corrections 0.05911 Final wR= 0.07265 Final frame scales: Min= 0.7502 Max= 1.1594 Final absorption correction factors: Amin= 0.4105 Amax= 1.5861 PROFFIT INFO: Inet (after scale3 abspack): min=-1144.8654 max=1375835.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=40.8394 max=24673.4160 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/104 5159 reflections read from tmp file 223 reflections are rejected (222 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 4 7 6 2 6 8 10 194 Initial Chi^2= 0.50691 Cycle 1, Chi^2= 1.02297 Current error model SIG(F2)^2 = 62.39*I_RAW + 9.75*I_BACK+(0.03735*)^2 Cycle 2, Chi^2= 1.01673 Current error model SIG(F2)^2 = 76.31*I_RAW + 6.96*I_BACK+(0.03045*)^2 Cycle 3, Chi^2= 1.00766 Current error model SIG(F2)^2 = 82.03*I_RAW + 6.02*I_BACK+(0.02852*)^2 Cycle 4, Chi^2= 1.00269 Current error model SIG(F2)^2 = 84.06*I_RAW + 5.72*I_BACK+(0.02802*)^2 Cycle 5, Chi^2= 1.00083 Current error model SIG(F2)^2 = 84.70*I_RAW + 5.63*I_BACK+(0.02789*)^2 Cycle 6, Chi^2= 1.00025 Current error model SIG(F2)^2 = 84.89*I_RAW + 5.61*I_BACK+(0.02785*)^2 Final Chi^2= 1.00025 Final error model SIG(F2)^2 = 84.89*I_RAW + 5.61*I_BACK+(0.02785*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1375835- 125171 515 408562.97 29.79 100.00 125035- 3680 515 31633.22 13.36 100.00 3676- 2188 515 2853.14 6.35 100.00 2171- 1220 515 1608.92 4.12 70.87 1220- 824 515 1005.23 2.86 30.10 823- 551 515 685.13 2.47 16.89 550- 355 515 448.57 2.04 9.51 355- 165 515 260.96 1.54 3.88 165- 26 515 90.43 0.78 0.39 26- -1145 524 -121.09 -0.49 0.00 ------------------------------------------------------------------------------------ 1375835- -1145 5159 44624.55 6.27 43.09 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 515 112145.04 10.13 72.23 1.73- 1.26 515 87607.23 9.58 65.05 1.26- 1.09 515 60594.19 8.16 71.84 1.09- 0.97 515 53768.65 6.66 39.03 0.97- 0.88 515 11318.51 4.25 50.49 0.88- 0.81 515 56048.50 8.06 46.60 0.81- 0.76 515 17987.25 3.80 21.55 0.76- 0.71 515 20052.26 4.86 22.52 0.71- 0.67 515 23807.30 5.51 33.59 0.67- 0.63 524 3632.95 1.77 8.59 ------------------------------------------------------------------------------------ 6.00- 0.63 5159 44624.55 6.27 43.09 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 515 112145.04 10.13 72.23 6.00- 1.26 1030 99876.13 9.85 68.64 6.00- 1.09 1545 86782.15 9.29 69.71 6.00- 0.97 2060 78528.78 8.63 62.04 6.00- 0.88 2575 65086.72 7.75 59.73 6.00- 0.81 3090 63580.35 7.81 57.54 6.00- 0.76 3605 57067.05 7.23 52.40 6.00- 0.71 4120 52440.20 6.94 48.67 6.00- 0.67 4635 49258.77 6.78 46.99 6.00- 0.63 5159 44624.55 6.27 43.09 ------------------------------------------------------------------------------------ 6.00- 0.63 5159 44624.55 6.27 43.09 Scale applied to data: s=0.726831 (maximum obs:1375835.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.059; Rsigma 0.038: data 5159 -> merged 240 With outlier rejection... Rint 0.052; Rsigma 0.038: data 5138 -> merged 240 Rejected total: 21, method kkm 15, method Blessing 6 Completeness direct cell (a, b, c) = (10.421, 10.421, 10.421), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627245, 6.016319 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.43 - 1.59 21 21 28.38 100.00 596 1.57 - 1.20 21 21 29.43 100.00 618 1.20 - 1.02 21 21 27.48 100.00 577 1.02 - 0.91 21 21 26.33 100.00 553 0.91 - 0.85 21 21 23.14 100.00 486 0.84 - 0.79 21 21 22.81 100.00 479 0.78 - 0.74 21 21 21.71 100.00 456 0.74 - 0.71 21 21 17.95 100.00 377 0.71 - 0.68 21 21 20.33 100.00 427 0.68 - 0.65 23 23 17.09 100.00 393 --------------------------------------------------------------- 10.43 - 0.65 212 212 23.41 100.00 4962 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:16:53 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.415002 10.431108 10.415611 89.9927 89.9710 90.0016 5138 Reflections read from file xs2212a.hkl 5107 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.27 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2564 0 3391 3386 5107 N (int>3sigma) = 0 0 0 0 1179 0 1550 1532 2207 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.2 31.1 32.1 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.4 6.3 6.3 Lattice type: F chosen Volume: 1131.55 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.363 7.367 7.370 60.02 60.04 90.00 Niggli form: a.a = 54.212 b.b = 54.267 c.c = 54.316 b.c = 27.132 a.c = 27.103 a.b = 0.003 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.169 CUBIC F-lattice R(int) = 0.052 [ 4876] Vol = 1131.6 Cell: 10.416 10.415 10.431 90.00 90.01 90.03 Volume: 1131.55 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.121 TETRAGONAL I-lattice R(int) = 0.050 [ 4491] Vol = 565.8 Cell: 7.370 7.370 10.416 90.02 89.97 89.91 Volume: 565.78 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.061 TETRAGONAL I-lattice R(int) = 0.051 [ 4490] Vol = 565.8 Cell: 7.363 7.367 10.431 90.00 89.99 90.00 Volume: 565.78 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.063 ORTHORHOMBIC F-lattice R(int) = 0.050 [ 4437] Vol = 1131.6 Cell: 10.416 10.415 10.431 90.00 90.01 89.97 Volume: 1131.55 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.135 ORTHORHOMBIC I-lattice R(int) = 0.050 [ 4418] Vol = 565.8 Cell: 10.416 7.370 7.370 89.91 89.97 90.02 Volume: 565.78 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.004 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4420] Vol = 565.8 Cell: 7.363 7.367 10.431 90.00 90.01 90.00 Volume: 565.78 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.059 MONOCLINIC I-lattice R(int) = 0.048 [ 3893] Vol = 565.8 Cell: 7.370 10.415 7.371 90.02 90.09 90.02 Volume: 565.78 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.057 MONOCLINIC I-lattice R(int) = 0.047 [ 3898] Vol = 565.8 Cell: 7.370 10.416 7.370 90.03 90.09 90.02 Volume: 565.78 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.004 MONOCLINIC I-lattice R(int) = 0.046 [ 3875] Vol = 565.8 Cell: 7.367 7.363 10.431 89.99 90.00 90.00 Volume: 565.78 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.003 MONOCLINIC I-lattice R(int) = 0.046 [ 3890] Vol = 565.8 Cell: 7.363 7.367 10.431 90.00 90.01 90.00 Volume: 565.78 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 2848] Vol = 282.9 Cell: 7.363 7.367 7.370 60.02 60.04 90.00 Volume: 282.89 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -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 2564 0 3393 3386 5107 N (int>3sigma) = 0 0 0 0 1179 0 1554 1532 2207 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.6 31.1 32.1 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.3 6.3 6.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.131 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 37 37 379 1005 N I>3s 2 2 2 550 0.0 0.0 0.0 2.0 0.9 0.9 0.3 5.2 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 0.051 4525 Fd-3m 1 1 227 C N N N N 37 2284 0.052 4587 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415611 10.415002 10.431108 90.0016 90.0073 90.0290 ZERR 5.00 0.001216 0.001494 0.001654 0.0122 0.0112 0.0106 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1219514- 135741 514 505 26 19.4 407656.10 29.78 0.047 0.060 115803- 3353 584 580 26 22.3 28501.96 12.50 0.068 0.078 3207- 1510 747 743 26 28.6 2356.69 5.76 0.124 0.178 1417- 902 645 645 26 24.8 1113.75 2.86 0.225 0.294 893- 529 635 635 26 24.4 692.97 2.42 0.288 0.390 528- 321 616 616 26 23.7 408.63 1.88 0.398 0.533 321- 172 510 510 26 19.6 246.11 1.33 0.565 0.845 171- 39 465 465 26 17.9 75.49 0.56 0.888 2.523 37- -386 443 439 32 13.7 -23.79 -0.03 0.966 2.689 ------------------------------------------------------------------------------------------- 1219514- -386 5159 5138 240 21.4 43929.31 6.23 0.052 0.066 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-1.45 767 762 26 29.3 123693.13 11.18 0.048 0.060 0.030 1.39-1.09 791 790 26 30.4 46070.04 7.25 0.045 0.057 0.036 1.06-0.94 661 658 26 25.3 41461.36 5.65 0.045 0.054 0.037 0.92-0.85 620 618 26 23.8 44914.66 7.45 0.052 0.067 0.042 0.84-0.78 604 603 26 23.2 26317.59 5.07 0.062 0.085 0.047 0.78-0.73 515 515 26 19.8 7937.00 2.88 0.082 0.098 0.079 0.73-0.69 545 543 27 20.1 20714.91 4.84 0.073 0.086 0.059 0.68-0.66 470 467 27 17.3 15642.33 3.99 0.079 0.106 0.066 0.65-0.63 186 182 30 6.1 8297.95 2.39 0.073 0.074 0.084 ------------------------------------------------------------------------------------------------------ inf-0.63 5159 5138 240 21.4 43929.31 6.23 0.052 0.066 0.038 inf-0.65 4977 4960 211 23.5 45278.79 6.39 0.051 0.065 0.038 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-1.45 762 26 26 100.0 29.3 123693.13 61.64 0.048 0.007 1.39-1.09 790 26 26 100.0 30.4 46070.04 36.97 0.045 0.008 1.06-0.94 658 26 26 100.0 25.3 41461.36 29.61 0.045 0.008 0.92-0.85 618 26 26 100.0 23.8 44914.66 36.26 0.052 0.009 0.84-0.78 603 26 26 100.0 23.2 26317.59 23.49 0.062 0.010 0.78-0.73 515 26 26 100.0 19.8 7937.00 12.50 0.082 0.018 0.73-0.69 543 27 27 100.0 20.1 20714.91 21.23 0.073 0.014 0.68-0.66 467 27 27 100.0 17.3 15642.33 18.32 0.079 0.016 0.65-0.63 182 30 30 100.0 6.1 8297.95 5.70 0.073 0.038 -------------------------------------------------------------------------------------------- inf-0.63 5138 240 240 100.0 21.4 43929.31 31.10 0.052 0.010 inf-0.65 4960 211 211 100.0 23.5 45278.79 32.04 0.051 0.009 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066078 0.014932 0.006903 ( 0.000010 0.000010 0.000010 ) -0.016067 0.064755 0.013200 ( 0.000010 0.000011 0.000010 ) -0.003705 -0.014415 0.066450 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004638 -0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000000 0.004624 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000000 0.004638 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066078 0.014932 0.006903 ( 0.000010 0.000010 0.000010 ) -0.016067 0.064755 0.013200 ( 0.000010 0.000011 0.000010 ) -0.003705 -0.014415 0.066450 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4150(15) 10.4310(17) 10.4156(12) 89.999(11) 89.974(11) 89.996(12) V = 1131.5(3) unit cell: 10.4205(4) 10.4205(4) 10.4205(4) 90.0 90.0 90.0 V = 1131.54(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.174) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.174) Run 5 Omega scan: (-6.000 - 96.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.174) PROFFIT INFO: signal sum: min=-775.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-679.7787 max=1265214.6783 PROFFIT INFO: background sum: min=-55.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=383.0000 max=6324.0000 PROFFIT INFO: num of signal pixels: min=41 max=555 PROFFIT INFO: Inet: min=-1087.6460 max=2024343.3750 PROFFIT INFO: sig(Inet): min=52.2346 max=30600.2930 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=218.80 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 858 3424 5260 6340 6842 7962 8676 9090 9758 10204 10318 Percent 8.3 33.2 51.0 61.4 66.3 77.2 84.1 88.1 94.6 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5159 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 5159 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2024343- 133510 515 434984.49 78.40 100.00 133403- 4275 515 32058.14 20.44 100.00 4270- 2219 515 3031.49 7.36 98.25 2209- 1298 515 1687.46 3.99 54.56 1297- 873 515 1063.65 2.44 18.06 871- 576 515 713.40 1.77 7.96 575- 365 515 463.97 1.30 6.02 364- 168 515 266.20 0.78 1.36 168- 25 515 90.17 0.31 0.00 25- -1088 524 -122.43 -0.23 0.00 ------------------------------------------------------------------------------------ 2024343- -1088 5159 47340.71 11.64 38.55 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 515 117843.92 15.44 68.74 1.73- 1.26 515 92389.65 21.50 61.36 1.26- 1.09 515 63808.22 19.07 66.80 1.09- 0.97 515 57940.03 15.55 36.50 0.97- 0.88 515 12984.33 5.85 42.14 0.88- 0.81 515 58412.36 16.09 39.42 0.81- 0.76 515 19312.89 5.85 18.25 0.76- 0.71 515 21739.70 7.02 17.28 0.71- 0.67 515 25938.37 8.31 29.13 0.67- 0.63 524 3798.57 1.85 6.49 ------------------------------------------------------------------------------------ 6.00- 0.63 5159 47340.71 11.64 38.55 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:16:53 2019 Sorting 5159 observations 43 unique observations with > 7.00 F2/sig(F2) 5159 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 101 514 Total number of frames 514 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 12 frame = 1 scale 5159 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 Total number of frames 45 1267 observations > 7.00 F2/sig(F2) 1267 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 Total number of frames 45 Removing 'redundancy=1' reflections Average redundancy: 23.0 (Out of 1267 removed 3 = 1264, unique = 55) 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 1264 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 Total number of frames 45 55 unique data precomputed (should be 55) 55 unique data with 1264 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.0 (Out of 1264 removed 0 = 1264, unique = 55) 55 unique data precomputed (should be 55) 55 unique data with 1264 observations RMS deviation of equivalent data = 0.28638 Rint = 0.23448 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.23106, wR= 0.30900 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11181, wR= 0.16185, Acormin=0.515, Acormax=1.403, Acor_av=0.976 F test: Probability=1.000, F= 4.253 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09956, wR= 0.14605, Acormin=0.470, Acormax=1.465, Acor_av=0.938 F test: Probability=1.000, F= 1.258 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09828, wR= 0.15218, Acormin=0.532, Acormax=1.501, Acor_av=0.984 F test: Probability=0.641, F= 1.021 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08738, wR= 0.13232, Acormin=0.475, Acormax=1.625, Acor_av=0.950 F test: Probability=1.000, F= 1.288 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07923, wR= 0.12273, Acormin=0.536, Acormax=1.800, Acor_av=0.973 F test: Probability=0.999, F= 1.209 Final absorption model (ne=4, no=3): Rint= 0.07923, Acormin=0.536, Acormax=1.800, Acor_av=0.973 Combined refinement in use Rint: 0.23613 There are 45 active scales (one needs to be fixed) Refinement control: frame scale #41 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 68 pars with 2346 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.28638 Using Levenberg-Marquardt: 0.00010 New wR= 0.10984 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23448 with corrections 0.07479 Rint for all data: 0.23613 with corrections 0.07738 4 observations identified as outliers and rejected Cycle 2 wR= 0.09299 Using Levenberg-Marquardt: 0.00001 New wR= 0.07751 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23279 with corrections 0.05596 Rint for all data: 0.23613 with corrections 0.06262 3 observations identified as outliers and rejected Cycle 3 wR= 0.06977 Using Levenberg-Marquardt: 0.00000 New wR= 0.06767 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23001 with corrections 0.04690 Rint for all data: 0.23613 with corrections 0.05544 1 observations identified as outliers and rejected Cycle 4 wR= 0.06432 Using Levenberg-Marquardt: 0.00000 New wR= 0.06381 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22936 with corrections 0.04484 Rint for all data: 0.23613 with corrections 0.05338 1 observations identified as outliers and rejected Cycle 5 wR= 0.06022 Using Levenberg-Marquardt: 0.00000 New wR= 0.05860 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22903 with corrections 0.04245 Rint for all data: 0.23613 with corrections 0.05145 0 observations identified as outliers and rejected Final wR= 0.05860 Final frame scales: Min= 0.7354 Max= 1.1862 Final absorption correction factors: Amin= 0.3888 Amax= 1.5388 PROFFIT INFO: Inet (after scale3 abspack): min=-1135.1650 max=1323224.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.8803 max=25785.3535 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/104 5159 reflections read from tmp file 169 reflections are rejected (169 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 2 3 3 2 3 6 4 139 Initial Chi^2= 0.48334 Cycle 1, Chi^2= 1.01988 Current error model SIG(F2)^2 = 59.55*I_RAW + 10.82*I_BACK+(0.03061*)^2 Cycle 2, Chi^2= 1.01449 Current error model SIG(F2)^2 = 71.94*I_RAW + 8.00*I_BACK+(0.02596*)^2 Cycle 3, Chi^2= 1.00454 Current error model SIG(F2)^2 = 75.68*I_RAW + 7.34*I_BACK+(0.02527*)^2 Cycle 4, Chi^2= 1.00108 Current error model SIG(F2)^2 = 76.60*I_RAW + 7.20*I_BACK+(0.02519*)^2 Cycle 5, Chi^2= 1.00025 Current error model SIG(F2)^2 = 76.81*I_RAW + 7.16*I_BACK+(0.02517*)^2 Final Chi^2= 1.00025 Final error model SIG(F2)^2 = 76.81*I_RAW + 7.16*I_BACK+(0.02517*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1323225- 128362 515 407166.46 32.57 100.00 127291- 3651 515 31794.06 14.21 100.00 3651- 2180 515 2856.19 6.66 100.00 2175- 1224 515 1618.43 4.27 75.53 1224- 825 515 1011.38 2.98 35.73 825- 554 515 687.08 2.56 20.58 553- 354 515 449.62 2.08 10.87 354- 166 515 261.75 1.53 4.66 165- 26 515 90.38 0.77 0.39 26- -1135 524 -119.78 -0.49 0.00 ------------------------------------------------------------------------------------ 1323225- -1135 5159 44503.58 6.70 44.70 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 515 111527.12 10.84 73.20 1.73- 1.26 515 86533.53 10.31 65.63 1.26- 1.09 515 60604.67 8.74 73.40 1.09- 0.97 515 53535.08 7.17 39.81 0.97- 0.88 515 11410.72 4.47 53.59 0.88- 0.81 515 56201.93 8.68 48.54 0.81- 0.76 515 18050.37 4.03 22.72 0.76- 0.71 515 20143.91 5.13 25.24 0.71- 0.67 515 24067.38 5.87 35.34 0.67- 0.63 524 3674.58 1.84 10.11 ------------------------------------------------------------------------------------ 6.00- 0.63 5159 44503.58 6.70 44.70 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 515 111527.12 10.84 73.20 6.00- 1.26 1030 99030.32 10.58 69.42 6.00- 1.09 1545 86221.77 9.97 70.74 6.00- 0.97 2060 78050.10 9.27 63.01 6.00- 0.88 2575 64722.22 8.31 61.13 6.00- 0.81 3090 63302.17 8.37 59.03 6.00- 0.76 3605 56837.63 7.75 53.84 6.00- 0.71 4120 52250.91 7.42 50.27 6.00- 0.67 4635 49119.41 7.25 48.61 6.00- 0.63 5159 44503.58 6.70 44.70 ------------------------------------------------------------------------------------ 6.00- 0.63 5159 44503.58 6.70 44.70 Scale applied to data: s=0.755729 (maximum obs:1323224.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.051; Rsigma 0.035: data 5159 -> merged 162 With outlier rejection... Rint 0.044; Rsigma 0.035: data 5141 -> merged 162 Rejected total: 18, method kkm 10, method Blessing 8 Completeness direct cell (a, b, c) = (10.421, 10.421, 10.421), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627242, 6.016291 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.43 - 1.76 14 14 33.79 100.00 473 1.74 - 1.27 14 14 37.36 100.00 523 1.26 - 1.06 14 14 41.93 100.00 587 1.05 - 0.97 14 14 36.43 100.00 510 0.95 - 0.88 14 14 37.71 100.00 528 0.87 - 0.81 14 14 33.43 100.00 468 0.80 - 0.76 14 14 35.14 100.00 492 0.76 - 0.72 14 14 29.50 100.00 413 0.72 - 0.69 14 14 32.36 100.00 453 0.69 - 0.65 19 19 27.21 100.00 517 --------------------------------------------------------------- 10.43 - 0.65 145 145 34.23 100.00 4964 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:16:53 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.415002 10.431108 10.415611 89.9927 89.9710 90.0016 5138 Reflections read from file xs2212a.hkl 5107 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.27 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2564 0 3391 3386 5107 N (int>3sigma) = 0 0 0 0 1179 0 1550 1532 2207 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.2 31.1 32.1 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.4 6.3 6.3 Lattice type: F chosen Volume: 1131.55 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.363 7.367 7.370 60.02 60.04 90.00 Niggli form: a.a = 54.212 b.b = 54.267 c.c = 54.316 b.c = 27.132 a.c = 27.103 a.b = 0.003 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.169 CUBIC F-lattice R(int) = 0.052 [ 4876] Vol = 1131.6 Cell: 10.416 10.415 10.431 90.00 90.01 90.03 Volume: 1131.55 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.121 TETRAGONAL I-lattice R(int) = 0.050 [ 4491] Vol = 565.8 Cell: 7.370 7.370 10.416 90.02 89.97 89.91 Volume: 565.78 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.061 TETRAGONAL I-lattice R(int) = 0.051 [ 4490] Vol = 565.8 Cell: 7.363 7.367 10.431 90.00 89.99 90.00 Volume: 565.78 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.063 ORTHORHOMBIC F-lattice R(int) = 0.050 [ 4437] Vol = 1131.6 Cell: 10.416 10.415 10.431 90.00 90.01 89.97 Volume: 1131.55 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.135 ORTHORHOMBIC I-lattice R(int) = 0.050 [ 4418] Vol = 565.8 Cell: 10.416 7.370 7.370 89.91 89.97 90.02 Volume: 565.78 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.004 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4420] Vol = 565.8 Cell: 7.363 7.367 10.431 90.00 90.01 90.00 Volume: 565.78 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.059 MONOCLINIC I-lattice R(int) = 0.048 [ 3893] Vol = 565.8 Cell: 7.370 10.415 7.371 90.02 90.09 90.02 Volume: 565.78 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.057 MONOCLINIC I-lattice R(int) = 0.047 [ 3898] Vol = 565.8 Cell: 7.370 10.416 7.370 90.03 90.09 90.02 Volume: 565.78 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.004 MONOCLINIC I-lattice R(int) = 0.046 [ 3875] Vol = 565.8 Cell: 7.367 7.363 10.431 89.99 90.00 90.00 Volume: 565.78 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.003 MONOCLINIC I-lattice R(int) = 0.046 [ 3890] Vol = 565.8 Cell: 7.363 7.367 10.431 90.00 90.01 90.00 Volume: 565.78 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 2848] Vol = 282.9 Cell: 7.363 7.367 7.370 60.02 60.04 90.00 Volume: 282.89 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -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 2564 0 3393 3386 5107 N (int>3sigma) = 0 0 0 0 1179 0 1554 1532 2207 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.6 31.1 32.1 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.3 6.3 6.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.131 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 37 37 379 1005 N I>3s 2 2 2 550 0.0 0.0 0.0 2.0 0.9 0.9 0.3 5.2 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 0.051 4525 Fd-3m 1 1 227 C N N N N 37 2284 0.052 4587 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415611 10.415002 10.431108 90.0016 90.0073 90.0290 ZERR 5.00 0.001216 0.001494 0.001654 0.0122 0.0112 0.0106 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1218265- 98806 629 619 27 22.9 355607.36 30.80 0.041 0.050 81364- 1928 973 969 27 35.9 5522.42 8.96 0.077 0.082 1797- 821 1020 1018 27 37.7 1208.21 3.26 0.208 0.282 821- 347 1014 1013 27 37.5 538.00 2.13 0.351 0.492 346- 71 777 776 27 28.7 232.12 1.26 0.578 0.953 70- -171 746 746 27 27.6 11.19 0.20 0.957 3.457 ------------------------------------------------------------------------------------------- 1218265- -171 5159 5141 162 31.7 44239.57 6.68 0.044 0.054 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-1.27 998 994 27 36.8 101339.84 10.83 0.039 0.046 0.028 1.26-0.97 1067 1063 27 39.4 54913.17 7.74 0.039 0.048 0.032 0.97-0.81 954 952 27 35.3 36470.40 6.98 0.050 0.063 0.040 0.81-0.73 921 920 27 34.1 11534.81 3.30 0.061 0.077 0.059 0.73-0.67 768 765 27 28.3 27769.09 6.29 0.064 0.081 0.052 0.67-0.63 451 447 27 16.6 3928.22 1.94 0.103 0.073 0.125 ------------------------------------------------------------------------------------------------------ inf-0.63 5159 5141 162 31.7 44239.57 6.68 0.044 0.054 0.035 inf-0.65 4977 4962 144 34.5 45596.12 6.84 0.044 0.053 0.035 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-1.27 994 27 27 100.0 36.8 101339.84 63.92 0.039 0.007 1.26-0.97 1063 27 27 100.0 39.4 54913.17 45.97 0.039 0.006 0.97-0.81 952 27 27 100.0 35.3 36470.40 41.95 0.050 0.008 0.81-0.73 920 27 27 100.0 34.1 11534.81 18.10 0.061 0.012 0.73-0.67 765 27 27 100.0 28.3 27769.09 34.63 0.064 0.010 0.67-0.63 447 27 27 100.0 16.6 3928.22 8.30 0.103 0.031 -------------------------------------------------------------------------------------------- inf-0.63 5141 162 162 100.0 31.7 44239.57 38.75 0.044 0.008 inf-0.65 4962 144 144 100.0 34.5 45596.12 39.92 0.044 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:17:55 2019) ID: 3668; threads 40; handles 810; mem 514428.00 (1204692.00)kB; time: 1w 5d 0h 28m 43s MEMORY INFO: Memory PF:225.0, Ph:554.0, V:1176.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:502.4,peak PF: 700.2, WS: 471.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:227.0, Ph:556.0, V:1178.0; MEMORY INFO: Process info - Handles: 811, Memory: PF:504.2,peak PF: 700.2, WS: 472.8, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:17:55 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000014 0.000014 ) -0.003867 -0.014380 0.066544 ( 0.000015 0.000017 0.000016 ) 10.42433 ( 0.00234 ) 10.43788 ( 0.00220 ) 10.40727 ( 0.00243 ) 89.88512 ( 0.01809 ) 89.79539 ( 0.01860 ) 90.20497 ( 0.01796 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:17:56 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000014 0.000014 ) -0.003867 -0.014380 0.066544 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004633 0.000003 -0.000009 ( 0.000002 0.000001 0.000001 ) 0.000003 0.004619 -0.000005 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000005 0.004649 ( 0.000001 0.000001 0.000002 ) unit cell: 10.424(2) 10.438(2) 10.407(2) 89.885(18) 89.795(19) 90.205(18) V = 1132.4(4) unit cell: 10.4200(8) 10.4200(8) 10.4200(8) 90.0 90.0 90.0 V = 1131.38(15) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 219 peaks identified as outliers and rejected 219 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 219 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 219 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.920 ( 0.073) | 0.989 ( 0.122) | 1.032 ( 0.498) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.033 ( 0.124) | 1.027 ( 0.679) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.939 ( 0.170) | 0.931 ( 0.396) | 1.00- 0.88 | 22 | 0.960 ( 0.074) | 1.004 ( 0.125) | 1.180 ( 0.494) | 0.88- 0.79 | 22 | 0.984 ( 0.058) | 1.025 ( 0.139) | 1.235 ( 0.386) | 0.79- 0.70 | 22 | 0.979 ( 0.045) | 0.955 ( 0.108) | 1.275 ( 0.476) | 0.69- 0.63 | 21 | 0.945 ( 0.037) | 0.919 ( 0.082) | 1.330 ( 0.484) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 219 | 0.933 ( 0.193) | 0.945 ( 0.158) | 1.115 ( 0.916) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.87 | 25 | 0.945 ( 0.067) | 0.936 ( 0.094) | 1.074 ( 0.403) | 0.86- 0.73 | 25 | 0.958 ( 0.050) | 0.919 ( 0.091) | 1.335 ( 0.450) | 0.73- 0.63 | 29 | 0.929 ( 0.037) | 0.880 ( 0.095) | 1.340 ( 0.463) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 254 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.061 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 238 peaks identified as outliers and rejected 238 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 238 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 238 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.971 ( 0.056) | 1.002 ( 0.095) | 1.053 ( 0.488) | 0.88- 0.79 | 24 | 1.001 ( 0.051) | 1.003 ( 0.120) | 0.913 ( 0.347) | 0.79- 0.70 | 24 | 0.995 ( 0.043) | 0.995 ( 0.132) | 1.319 ( 0.485) | 0.69- 0.63 | 22 | 0.974 ( 0.053) | 0.912 ( 0.110) | 1.255 ( 0.524) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 238 | 0.949 ( 0.083) | 0.961 ( 0.132) | 1.035 ( 0.512) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb PROFFITPEAK info: 569 peaks in the peak location table UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000001 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) unit cell: 10.4202(10) 10.4202(10) 10.4202(10) 90.0 90.0 90.0 V = 1131.43(19) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 1 302 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000001 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) unit cell: 10.4202(10) 10.4202(10) 10.4202(10) 90.0 90.0 90.0 V = 1131.43(19) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | 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- 9.8 | 120 | 0.988 ( 0.040) | 1.032 ( 0.067) | 1.119 ( 0.482) | 9.8-14.5 | 120 | 0.994 ( 0.046) | 1.049 ( 0.070) | 1.126 ( 0.544) | 14.5-18.7 | 120 | 0.996 ( 0.193) | 1.033 ( 0.099) | 1.146 ( 1.014) | 18.7-23.4 | 120 | 0.968 ( 0.059) | 1.011 ( 0.081) | 0.915 ( 0.419) | 23.4-26.8 | 120 | 0.970 ( 0.062) | 1.000 ( 0.095) | 1.005 ( 0.446) | 26.9-32.0 | 120 | 0.945 ( 0.078) | 0.964 ( 0.105) | 0.945 ( 0.447) | 32.0-36.1 | 120 | 0.928 ( 0.156) | 0.926 ( 0.141) | 1.049 ( 0.675) | 36.1-38.7 | 120 | 0.884 ( 0.100) | 0.855 ( 0.135) | 1.014 ( 0.461) | 38.8-41.9 | 120 | 0.905 ( 0.099) | 0.882 ( 0.254) | 1.039 ( 0.479) | 41.9-50.1 | 124 | 0.864 ( 0.122) | 0.797 ( 0.142) | 0.932 ( 0.455) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1204 | 0.944 ( 0.116) | 0.954 ( 0.154) | 1.029 ( 0.574) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.14 e2 dimension: a=-0.0067 b=1.23 e3 dimension: a=0.0007 b=1.09 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 4496 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 14:18:12 2019 PROFFITMAIN - Started at Wed Aug 21 14:18:12 2019 OTKP changes: 955 2 4 5 OTKP changes: 955 2 4 5 OTKP changes: 955 2 4 5 No constraint UB - matrix: 0.066033 0.015001 0.006771 ( 0.000014 0.000016 0.000015 ) -0.016044 0.064688 0.013096 ( 0.000013 0.000015 0.000014 ) -0.003773 -0.014361 0.066571 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004632 0.000007 -0.000014 ( 0.000002 0.000001 0.000001 ) 0.000007 0.004616 -0.000007 ( 0.000001 0.000002 0.000002 ) -0.000014 -0.000007 0.004649 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015001 0.006771 ( 0.000014 0.000016 0.000015 ) -0.016044 0.064688 0.013096 ( 0.000013 0.000015 0.000014 ) -0.003773 -0.014361 0.066571 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000001 ) UB fit with 967 obs out of 1204 (total:1204,skipped:0) (80.32%) unit cell: 10.422(2) 10.440(2) 10.403(2) 89.910(19) 89.825(18) 90.085(18) V = 1131.9(4) unit cell: 10.4216(8) 10.4216(8) 10.4216(8) 90.0 90.0 90.0 V = 1131.89(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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 186 obs out of 219 (total:219,skipped:0) (84.93%) UB - matrix: 0.066501 0.011703 0.008961 ( 0.000032 0.000043 0.000036 ) -0.013687 0.065060 0.013250 ( 0.000031 0.000041 0.000034 ) -0.006054 -0.013932 0.065930 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.61(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 No constraint UB - matrix: 0.066497 0.011708 0.008954 ( 0.000032 0.000042 0.000035 ) -0.013711 0.065052 0.013255 ( 0.000032 0.000042 0.000035 ) -0.006056 -0.013931 0.065945 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004646 -0.000029 0.000014 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004563 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000048 0.004605 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066497 0.011708 0.008954 ( 0.000032 0.000042 0.000035 ) -0.013711 0.065052 0.013255 ( 0.000032 0.000042 0.000035 ) -0.006056 -0.013931 0.065945 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 219 (total:219,skipped:0) (86.30%) unit cell: 10.406(5) 10.501(6) 10.453(6) 90.61(5) 90.18(4) 89.64(4) V = 1142(1) unit cell: 10.4532(19) 10.4532(19) 10.4532(19) 90.0 90.0 90.0 V = 1142.2(3) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.138) HKL list info: 1310 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066497 0.011708 0.008954 ( 0.000032 0.000042 0.000035 ) -0.013711 0.065052 0.013255 ( 0.000032 0.000042 0.000035 ) -0.006055 -0.013931 0.065945 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004646 -0.000029 0.000014 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004563 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000048 0.004605 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066497 0.011708 0.008954 ( 0.000032 0.000042 0.000035 ) -0.013711 0.065052 0.013255 ( 0.000032 0.000042 0.000035 ) -0.006055 -0.013931 0.065945 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 219 (total:219,skipped:0) (86.30%) unit cell: 10.406(5) 10.501(6) 10.453(6) 90.61(5) 90.18(4) 89.64(4) V = 1142(1) unit cell: 10.4532(19) 10.4532(19) 10.4532(19) 90.0 90.0 90.0 V = 1142.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 219 (total:219,skipped:0) (92.69%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068141 -0.000274 0.000126 ( 0.000028 0.000036 0.000029 ) -0.000077 0.067601 0.000628 ( 0.000032 0.000041 0.000033 ) -0.000032 -0.000065 0.067956 ( 0.000023 0.000030 0.000024 ) M - matrix: 0.004643 -0.000024 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000024 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000038 0.004618 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068141 -0.000274 0.000126 ( 0.000028 0.000036 0.000029 ) -0.000077 0.067601 0.000628 ( 0.000032 0.000041 0.000033 ) -0.000032 -0.000065 0.067956 ( 0.000023 0.000030 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 205 obs out of 219 (total:219,skipped:0) (93.61%) unit cell: 10.409(4) 10.493(6) 10.438(4) 90.47(4) 90.08(3) 89.70(4) V = 1140.0(9) unit cell: 10.4464(13) 10.4464(13) 10.4464(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.066336 0.014186 0.006779 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064704 0.012861 ( 0.000017 0.000022 0.000023 ) -0.004076 -0.014197 0.066901 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.393(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4047(5) 10.4047(5) 10.4047(5) 90.0 90.0 90.0 V = 1126.40(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) UB - matrix: 0.065854 0.015173 0.006787 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064731 0.013264 ( 0.000016 0.000011 0.000016 ) -0.003661 -0.014497 0.066469 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004608 0.000012 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000012 0.004630 -0.000002 ( 0.000001 0.000002 0.000001 ) -0.000010 -0.000002 0.004640 ( 0.000002 0.000001 0.000003 ) unit cell: 10.449(3) 10.4236(19) 10.413(3) 89.976(19) 89.88(2) 90.149(18) V = 1134.1(5) OTKP changes: 238 1 1 1 OTKP changes: 238 1 1 1 OTKP changes: 238 1 1 1 No constraint UB - matrix: 0.065827 0.015155 0.006804 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064737 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003668 -0.014467 0.066449 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004604 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065827 0.015155 0.006804 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064737 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003668 -0.014467 0.066449 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000000 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 10.453(3) 10.4243(19) 10.416(3) 90.000(19) 89.89(2) 90.140(18) V = 1135.0(5) unit cell: 10.4310(6) 10.4310(6) 10.4310(6) 90.0 90.0 90.0 V = 1134.96(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.173) HKL list info: 1274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065827 0.015155 0.006804 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064737 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003668 -0.014467 0.066449 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004604 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065827 0.015155 0.006804 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064737 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003668 -0.014467 0.066449 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000000 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 10.453(3) 10.4243(19) 10.416(3) 90.000(19) 89.89(2) 90.140(18) V = 1135.0(5) unit cell: 10.4310(6) 10.4310(6) 10.4310(6) 90.0 90.0 90.0 V = 1134.96(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 238 obs out of 238 (total:238,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) ******* No constraint UB - matrix: 0.065827 0.015155 0.006804 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064737 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003668 -0.014467 0.066449 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004604 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065827 0.015155 0.006804 ( 0.000019 0.000013 0.000019 ) -0.016056 0.064737 0.013257 ( 0.000017 0.000011 0.000016 ) -0.003668 -0.014467 0.066449 ( 0.000020 0.000014 0.000020 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000000 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 10.453(3) 10.4243(19) 10.416(3) 90.000(19) 89.89(2) 90.140(18) V = 1135.0(5) unit cell: 10.4310(6) 10.4310(6) 10.4310(6) 90.0 90.0 90.0 V = 1134.96(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066076 0.015220 0.006574 ( 0.000014 0.000018 0.000015 ) -0.016357 0.064708 0.012945 ( 0.000012 0.000016 0.000014 ) -0.003384 -0.014183 0.066473 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004645 -0.000005 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004620 -0.000005 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000005 0.004629 ( 0.000001 0.000001 0.000002 ) unit cell: 10.407(2) 10.436(2) 10.4247(18) 89.937(16) 89.971(16) 89.941(18) V = 1132.2(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066045 0.015195 0.006551 ( 0.000013 0.000018 0.000015 ) -0.016307 0.064679 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003373 -0.014171 0.066486 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004639 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004615 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004631 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066045 0.015195 0.006551 ( 0.000013 0.000018 0.000015 ) -0.016307 0.064679 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003373 -0.014171 0.066486 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.414(2) 10.441(2) 10.4226(18) 89.948(16) 89.964(16) 89.958(18) V = 1133.2(4) unit cell: 10.4258(5) 10.4258(5) 10.4258(5) 90.0 90.0 90.0 V = 1133.25(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.173) HKL list info: 1300 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066045 0.015195 0.006551 ( 0.000013 0.000018 0.000015 ) -0.016307 0.064679 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003373 -0.014171 0.066486 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004639 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004615 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004631 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066045 0.015195 0.006551 ( 0.000013 0.000018 0.000015 ) -0.016307 0.064679 0.012963 ( 0.000012 0.000016 0.000013 ) -0.003373 -0.014171 0.066486 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.414(2) 10.441(2) 10.4226(18) 89.948(16) 89.964(16) 89.958(18) V = 1133.2(4) unit cell: 10.4258(5) 10.4258(5) 10.4258(5) 90.0 90.0 90.0 V = 1133.25(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068097 -0.000048 -0.000033 ( 0.000011 0.000015 0.000012 ) 0.000002 0.067949 -0.000048 ( 0.000013 0.000018 0.000015 ) 0.000006 0.000008 0.068054 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004637 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004617 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004631 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068097 -0.000048 -0.000033 ( 0.000011 0.000015 0.000012 ) 0.000002 0.067949 -0.000048 ( 0.000013 0.000018 0.000015 ) 0.000006 0.000008 0.068054 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.4160(17) 10.439(3) 10.4226(16) 89.966(16) 89.978(13) 89.961(17) V = 1133.2(4) unit cell: 10.4257(5) 10.4257(5) 10.4257(5) 90.0 90.0 90.0 V = 1133.24(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 249 obs out of 271 (total:271,skipped:0) (91.88%) UB - matrix: 0.065944 0.015337 0.006313 ( 0.000017 0.000013 0.000013 ) -0.016318 0.064755 0.013392 ( 0.000022 0.000017 0.000017 ) -0.003164 -0.014532 0.066439 ( 0.000032 0.000024 0.000024 ) M - matrix: 0.004625 0.000001 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000001 0.004640 -0.000001 ( 0.000002 0.000002 0.000002 ) -0.000012 -0.000001 0.004633 ( 0.000002 0.000002 0.000003 ) unit cell: 10.430(3) 10.413(3) 10.420(4) 89.98(2) 89.85(3) 90.01(2) V = 1131.7(6) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.065936 0.015334 0.006290 ( 0.000016 0.000012 0.000013 ) -0.016330 0.064729 0.013400 ( 0.000018 0.000013 0.000014 ) -0.002845 -0.014641 0.066438 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.004622 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004639 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065936 0.015334 0.006290 ( 0.000016 0.000012 0.000013 ) -0.016330 0.064729 0.013400 ( 0.000018 0.000013 0.000014 ) -0.002845 -0.014641 0.066438 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.433(2) 10.414(2) 10.4206(19) 89.890(16) 90.085(17) 89.947(18) V = 1132.1(4) unit cell: 10.4223(6) 10.4223(6) 10.4223(6) 90.0 90.0 90.0 V = 1132.13(11) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.173) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065936 0.015334 0.006290 ( 0.000016 0.000012 0.000013 ) -0.016330 0.064729 0.013400 ( 0.000018 0.000013 0.000014 ) -0.002845 -0.014641 0.066438 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.004622 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004639 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065936 0.015334 0.006290 ( 0.000016 0.000012 0.000013 ) -0.016330 0.064729 0.013400 ( 0.000018 0.000013 0.000014 ) -0.002845 -0.014641 0.066438 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.433(2) 10.414(2) 10.4206(19) 89.890(16) 90.085(17) 89.947(18) V = 1132.1(4) unit cell: 10.4223(6) 10.4223(6) 10.4223(6) 90.0 90.0 90.0 V = 1132.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068000 -0.000083 0.000062 ( 0.000017 0.000013 0.000013 ) 0.000051 0.068082 -0.000088 ( 0.000014 0.000010 0.000011 ) -0.000013 0.000007 0.068058 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000002 0.000003 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004635 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000003 -0.000006 0.004632 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068000 -0.000083 0.000062 ( 0.000017 0.000013 0.000013 ) 0.000051 0.068082 -0.000088 ( 0.000014 0.000010 0.000011 ) -0.000013 0.000007 0.068058 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.431(3) 10.4183(16) 10.4220(19) 89.931(14) 90.042(17) 89.973(16) V = 1132.6(4) unit cell: 10.4237(6) 10.4237(6) 10.4237(6) 90.0 90.0 90.0 V = 1132.58(11) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068105 0.000012 -0.000070 ( 0.000010 0.000010 0.000010 ) -0.000013 0.068000 0.000011 ( 0.000010 0.000011 0.000010 ) 0.000034 -0.000023 0.068102 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004638 -0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000000 0.004624 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000001 0.004638 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068105 0.000012 -0.000070 ( 0.000010 0.000010 0.000010 ) -0.000013 0.068000 0.000011 ( 0.000010 0.000011 0.000010 ) 0.000034 -0.000023 0.068102 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000000 ) UB fit with 1181 obs out of 1204 (total:1204,skipped:0) (98.09%) unit cell: 10.4148(15) 10.4308(16) 10.4153(12) 89.990(11) 89.969(11) 89.999(12) V = 1131.5(3) unit cell: 10.4203(4) 10.4203(4) 10.4203(4) 90.0 90.0 90.0 V = 1131.47(7) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 104 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof 5177 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:18:20 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.138) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.173) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.173) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.173) PROFFIT INFO: signal sum: min=-766.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-679.7435 max=1270674.5202 PROFFIT INFO: background sum: min=-55.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=383.0000 max=6324.0000 PROFFIT INFO: num of signal pixels: min=41 max=555 PROFFIT INFO: Inet: min=-1087.5897 max=2033079.2500 PROFFIT INFO: sig(Inet): min=52.0726 max=30646.9688 PROFFIT INFO: Inet/sig(Inet): min=-2.09 max=218.93 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 419 1721 2630 3179 3430 3996 4355 4563 4897 5120 5177 Percent 8.1 33.2 50.8 61.4 66.3 77.2 84.1 88.1 94.6 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5177 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 5177 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2033079- 133555 517 434025.89 78.29 100.00 133536- 4271 517 31567.00 20.30 100.00 4262- 2215 517 3032.34 7.37 98.26 2208- 1305 517 1690.81 3.99 54.16 1302- 876 517 1066.90 2.45 18.57 875- 578 517 714.59 1.77 7.93 577- 365 517 463.32 1.30 6.38 364- 169 517 265.02 0.77 1.16 168- 26 517 91.39 0.32 0.00 25- -1088 524 -121.47 -0.23 0.00 ------------------------------------------------------------------------------------ 2033079- -1088 5177 47215.49 11.62 38.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 517 117406.74 15.41 68.67 1.73- 1.26 517 92068.92 21.49 61.51 1.26- 1.09 517 63536.59 19.02 67.12 1.09- 0.97 517 57709.76 15.48 36.36 0.97- 0.88 517 15026.93 6.32 42.55 0.88- 0.81 517 56135.98 15.58 38.88 0.81- 0.76 517 19042.20 5.78 17.99 0.76- 0.71 517 22151.69 7.09 17.60 0.71- 0.67 517 25842.05 8.28 29.01 0.67- 0.63 524 3821.55 1.87 6.68 ------------------------------------------------------------------------------------ 6.00- 0.63 5177 47215.49 11.62 38.59 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:18:20 2019 Sorting 5177 observations 53 unique observations with > 7.00 F2/sig(F2) 5177 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 Total number of frames 516 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 5177 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 10 55 Total number of frames 55 1271 observations > 7.00 F2/sig(F2) 1271 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 10 55 Total number of frames 55 Removing 'redundancy=1' reflections Average redundancy: 18.9 (Out of 1271 removed 7 = 1264, unique = 67) 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 1264 observations in 5 runs Run # start # end # total # 1 0 10 11 2 0 10 22 3 0 10 33 4 0 10 44 5 0 10 55 Total number of frames 55 67 unique data precomputed (should be 67) 67 unique data with 1264 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 18.9 (Out of 1264 removed 0 = 1264, unique = 67) 67 unique data precomputed (should be 67) 67 unique data with 1264 observations RMS deviation of equivalent data = 0.28554 Rint = 0.23394 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.23052, wR= 0.30789 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11147, wR= 0.15998, Acormin=0.514, Acormax=1.404, Acor_av=0.974 F test: Probability=1.000, F= 4.259 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09894, wR= 0.14422, Acormin=0.471, Acormax=1.465, Acor_av=0.937 F test: Probability=1.000, F= 1.266 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09783, wR= 0.14990, Acormin=0.534, Acormax=1.504, Acor_av=0.982 F test: Probability=0.618, F= 1.018 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08638, wR= 0.13017, Acormin=0.478, Acormax=1.628, Acor_av=0.950 F test: Probability=1.000, F= 1.302 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07857, wR= 0.12057, Acormin=0.537, Acormax=1.800, Acor_av=0.973 F test: Probability=0.999, F= 1.202 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09697, wR= 0.14449, Acormin=0.444, Acormax=1.579, Acor_av=0.956 F test: Probability=0.000, F= 0.655 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08380, wR= 0.12832, Acormin=0.472, Acormax=1.634, Acor_av=0.938 F test: Probability=0.000, F= 0.875 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07575, wR= 0.11824, Acormin=0.522, Acormax=1.837, Acor_av=0.969 F test: Probability=0.854, F= 1.064 Trying model 9 (ne=6, no=5)... Results: Rint= 0.09652, wR= 0.13759, Acormin=0.182, Acormax=1.094, Acor_av=0.550 F test: Probability=0.000, F= 0.649 Final absorption model (ne=4, no=3): Rint= 0.07857, Acormin=0.537, Acormax=1.800, Acor_av=0.973 Combined refinement in use Rint: 0.23558 There are 55 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: 4, max odd order: 3 (24 parameters) Refinement control: 78 pars with 3081 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.28554 Using Levenberg-Marquardt: 0.00010 New wR= 0.09190 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23394 with corrections 0.06126 Rint for all data: 0.23558 with corrections 0.06398 1 observations identified as outliers and rejected Cycle 2 wR= 0.08522 Using Levenberg-Marquardt: 0.00001 New wR= 0.07786 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23382 with corrections 0.05340 Rint for all data: 0.23558 with corrections 0.05925 0 observations identified as outliers and rejected Cycle 3 wR= 0.07786 Using Levenberg-Marquardt: 0.00000 New wR= 0.07846 Using Levenberg-Marquardt: 0.00001 New wR= 0.07846 Using Levenberg-Marquardt: 0.00010 New wR= 0.07846 Using Levenberg-Marquardt: 0.00100 New wR= 0.07845 Using Levenberg-Marquardt: 0.01000 New wR= 0.07837 Using Levenberg-Marquardt: 0.10000 New wR= 0.07807 Using Levenberg-Marquardt: 1.00000 New wR= 0.07787 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23382 with corrections 0.05318 Rint for all data: 0.23558 with corrections 0.05893 Final wR= 0.07787 Final frame scales: Min= 0.7374 Max= 1.1319 Final absorption correction factors: Amin= 0.4057 Amax= 1.5489 PROFFIT INFO: Inet (after scale3 abspack): min=-1071.4766 max=1375511.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=40.7116 max=25533.6855 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/104 5177 reflections read from tmp file 217 reflections are rejected (216 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 6 6 1 5 9 9 195 Initial Chi^2= 0.49262 Cycle 1, Chi^2= 1.01986 Current error model SIG(F2)^2 = 61.72*I_RAW + 9.10*I_BACK+(0.03629*)^2 Cycle 2, Chi^2= 1.01638 Current error model SIG(F2)^2 = 75.01*I_RAW + 6.70*I_BACK+(0.02795*)^2 Cycle 3, Chi^2= 1.00747 Current error model SIG(F2)^2 = 80.33*I_RAW + 5.89*I_BACK+(0.02592*)^2 Cycle 4, Chi^2= 1.00221 Current error model SIG(F2)^2 = 82.00*I_RAW + 5.69*I_BACK+(0.02552*)^2 Cycle 5, Chi^2= 1.00055 Current error model SIG(F2)^2 = 82.43*I_RAW + 5.64*I_BACK+(0.02544*)^2 Cycle 6, Chi^2= 1.00013 Current error model SIG(F2)^2 = 82.53*I_RAW + 5.62*I_BACK+(0.02542*)^2 Final Chi^2= 1.00013 Final error model SIG(F2)^2 = 82.53*I_RAW + 5.62*I_BACK+(0.02542*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1375511- 125415 517 406950.13 31.90 100.00 125340- 3672 517 31218.04 13.70 100.00 3669- 2152 517 2844.70 6.48 100.00 2152- 1214 517 1610.23 4.17 72.92 1214- 824 517 1007.06 2.90 31.53 824- 550 517 686.16 2.51 18.57 550- 352 517 448.51 2.08 10.64 352- 165 517 260.52 1.55 4.06 164- 27 517 91.39 0.80 0.58 27- -1071 524 -120.59 -0.49 0.00 ------------------------------------------------------------------------------------ 1375511- -1071 5177 44439.28 6.55 43.77 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 517 111078.02 10.63 72.53 1.73- 1.26 517 87334.22 10.08 65.57 1.26- 1.09 517 60229.39 8.56 72.73 1.09- 0.97 517 53503.44 7.00 39.26 0.97- 0.88 517 12795.14 4.55 51.64 0.88- 0.81 517 54465.96 8.29 47.58 0.81- 0.76 517 17733.56 3.90 22.24 0.76- 0.71 517 20324.29 5.06 23.02 0.71- 0.67 517 23777.74 5.67 34.24 0.67- 0.63 524 3702.63 1.83 9.35 ------------------------------------------------------------------------------------ 6.00- 0.63 5177 44439.28 6.55 43.77 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 517 111078.02 10.63 72.53 6.00- 1.26 1034 99206.12 10.35 69.05 6.00- 1.09 1551 86213.88 9.76 70.28 6.00- 0.97 2068 78036.27 9.07 62.52 6.00- 0.88 2585 64988.04 8.16 60.35 6.00- 0.81 3102 63234.36 8.18 58.22 6.00- 0.76 3619 56734.25 7.57 53.08 6.00- 0.71 4136 52183.00 7.26 49.32 6.00- 0.67 4653 49026.86 7.08 47.65 6.00- 0.63 5177 44439.28 6.55 43.77 ------------------------------------------------------------------------------------ 6.00- 0.63 5177 44439.28 6.55 43.77 Scale applied to data: s=0.727002 (maximum obs:1375511.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.059; Rsigma 0.036: data 5177 -> merged 240 With outlier rejection... Rint 0.049; Rsigma 0.036: data 5152 -> merged 240 Rejected total: 25, method kkm 18, method Blessing 7 Completeness direct cell (a, b, c) = (10.420, 10.420, 10.420), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627229, 6.016173 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.43 - 1.59 21 21 28.38 100.00 596 1.57 - 1.20 21 21 29.52 100.00 620 1.20 - 1.02 21 21 27.52 100.00 578 1.02 - 0.91 21 21 26.33 100.00 553 0.91 - 0.85 21 21 23.33 100.00 490 0.84 - 0.79 21 21 22.95 100.00 482 0.78 - 0.74 21 21 21.81 100.00 458 0.74 - 0.71 21 21 18.05 100.00 379 0.71 - 0.68 21 21 20.33 100.00 427 0.68 - 0.65 23 23 17.09 100.00 393 --------------------------------------------------------------- 10.43 - 0.65 212 212 23.47 100.00 4976 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:18:21 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.414817 10.430843 10.415300 89.9898 89.9692 89.9991 5152 Reflections read from file xs2212a.hkl 5122 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.52 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2574 0 3398 3395 5122 N (int>3sigma) = 0 0 0 0 1207 0 1568 1553 2246 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.7 30.5 31.7 Mean int/sigma = 0.0 0.0 0.0 0.0 4.2 0.0 6.7 6.5 6.5 Lattice type: F chosen Volume: 1131.47 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.363 7.367 7.370 60.02 60.04 90.00 Niggli form: a.a = 54.208 b.b = 54.266 c.c = 54.311 b.c = 27.129 a.c = 27.101 a.b = 0.003 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.170 CUBIC F-lattice R(int) = 0.049 [ 4891] Vol = 1131.5 Cell: 10.415 10.415 10.431 90.00 90.01 90.03 Volume: 1131.47 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.121 TETRAGONAL I-lattice R(int) = 0.047 [ 4506] Vol = 565.7 Cell: 7.370 7.370 10.415 90.01 89.97 89.91 Volume: 565.73 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.064 TETRAGONAL I-lattice R(int) = 0.049 [ 4505] Vol = 565.7 Cell: 7.363 7.367 10.431 89.99 89.99 90.00 Volume: 565.73 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.064 ORTHORHOMBIC F-lattice R(int) = 0.047 [ 4452] Vol = 1131.5 Cell: 10.415 10.415 10.431 90.00 90.01 89.97 Volume: 1131.47 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.136 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4432] Vol = 565.7 Cell: 10.415 7.370 7.370 89.91 89.97 90.01 Volume: 565.73 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.006 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 4435] Vol = 565.7 Cell: 7.363 7.367 10.431 90.01 90.01 90.00 Volume: 565.73 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.062 MONOCLINIC I-lattice R(int) = 0.045 [ 3908] Vol = 565.7 Cell: 7.370 10.415 7.371 90.02 90.09 90.02 Volume: 565.73 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.060 MONOCLINIC I-lattice R(int) = 0.045 [ 3912] Vol = 565.7 Cell: 7.370 10.415 7.370 90.03 90.09 90.01 Volume: 565.73 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.004 MONOCLINIC I-lattice R(int) = 0.043 [ 3890] Vol = 565.7 Cell: 7.367 7.363 10.431 89.99 90.01 90.00 Volume: 565.73 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.005 MONOCLINIC I-lattice R(int) = 0.043 [ 3905] Vol = 565.7 Cell: 7.363 7.367 10.431 89.99 90.01 90.00 Volume: 565.73 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.038 [ 2862] Vol = 282.9 Cell: 7.363 7.367 7.370 60.02 60.04 90.00 Volume: 282.87 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -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 2574 0 3406 3395 5122 N (int>3sigma) = 0 0 0 0 1207 0 1581 1553 2246 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.1 30.5 31.7 Mean int/sigma = 0.0 0.0 0.0 0.0 4.2 0.0 6.6 6.5 6.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.113 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 37 37 380 1007 N I>3s 2 2 2 562 0.0 0.0 0.0 1.9 0.9 0.9 0.3 5.3 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 0.049 4539 Fd-3m 1 1 227 C N N N N 37 2284 0.049 4601 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415300 10.414817 10.430843 89.9991 90.0102 90.0308 ZERR 5.00 0.001211 0.001489 0.001644 0.0122 0.0111 0.0106 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1211304- 136221 514 502 26 19.3 404930.34 31.86 0.045 0.056 115804- 3374 586 581 26 22.3 28546.58 12.85 0.068 0.076 3201- 1513 751 747 26 28.7 2356.03 5.87 0.124 0.176 1416- 897 651 651 26 25.0 1112.55 2.90 0.226 0.297 892- 534 637 637 26 24.5 695.90 2.46 0.287 0.384 532- 326 589 589 26 22.7 411.77 1.89 0.402 0.527 324- 173 522 522 26 20.1 254.79 1.41 0.547 0.799 149- 33 498 498 26 19.2 75.09 0.57 0.874 2.530 32- -341 429 425 32 13.3 -25.15 -0.03 0.975 2.913 ------------------------------------------------------------------------------------------- 1211304- -341 5177 5152 240 21.5 43321.11 6.49 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-1.45 770 763 26 29.3 121635.04 11.72 0.044 0.054 0.028 1.39-1.09 794 792 26 30.5 44939.14 7.53 0.045 0.053 0.034 1.06-0.94 661 657 26 25.3 40781.83 5.89 0.042 0.052 0.035 0.92-0.85 625 623 26 24.0 44680.06 7.77 0.051 0.066 0.039 0.84-0.78 608 607 26 23.3 25976.42 5.22 0.057 0.077 0.045 0.78-0.73 541 541 27 20.0 13907.55 3.95 0.072 0.092 0.061 0.72-0.69 522 520 26 20.0 15392.09 4.10 0.077 0.088 0.064 0.68-0.66 470 467 27 17.3 15688.76 4.11 0.077 0.103 0.064 0.65-0.63 186 182 30 6.1 8458.67 2.52 0.070 0.066 0.082 ------------------------------------------------------------------------------------------------------ inf-0.63 5177 5152 240 21.5 43321.11 6.49 0.049 0.062 0.036 inf-0.65 4995 4974 211 23.6 44639.39 6.64 0.049 0.061 0.036 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-1.45 763 26 26 100.0 29.3 121635.04 64.37 0.044 0.006 1.39-1.09 792 26 26 100.0 30.5 44939.14 38.33 0.045 0.008 1.06-0.94 657 26 26 100.0 25.3 40781.83 30.63 0.042 0.008 0.92-0.85 623 26 26 100.0 24.0 44680.06 37.81 0.051 0.009 0.84-0.78 607 26 26 100.0 23.3 25976.42 24.06 0.057 0.010 0.78-0.73 541 27 27 100.0 20.0 13907.55 17.78 0.072 0.014 0.72-0.69 520 26 26 100.0 20.0 15392.09 17.38 0.077 0.015 0.68-0.66 467 27 27 100.0 17.3 15688.76 18.82 0.077 0.016 0.65-0.63 182 30 30 100.0 6.1 8458.67 6.00 0.070 0.037 -------------------------------------------------------------------------------------------- inf-0.63 5152 240 240 100.0 21.5 43321.11 32.28 0.049 0.009 inf-0.65 4974 211 211 100.0 23.6 44639.39 33.25 0.049 0.009 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066078 0.014932 0.006900 ( 0.000010 0.000010 0.000010 ) -0.016071 0.064755 0.013199 ( 0.000010 0.000011 0.000011 ) -0.003704 -0.014414 0.066453 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004638 -0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000001 0.004624 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000000 0.004638 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066078 0.014932 0.006900 ( 0.000010 0.000010 0.000010 ) -0.016071 0.064755 0.013199 ( 0.000010 0.000011 0.000011 ) -0.003704 -0.014414 0.066453 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4148(15) 10.4310(17) 10.4153(12) 89.999(11) 89.972(11) 89.993(12) V = 1131.5(3) unit cell: 10.4204(4) 10.4204(4) 10.4204(4) 90.0 90.0 90.0 V = 1131.49(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.138) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.173) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.173) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.173) PROFFIT INFO: signal sum: min=-766.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-679.7435 max=1270674.5202 PROFFIT INFO: background sum: min=-55.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=383.0000 max=6324.0000 PROFFIT INFO: num of signal pixels: min=41 max=555 PROFFIT INFO: Inet: min=-1087.5897 max=2033079.2500 PROFFIT INFO: sig(Inet): min=52.0726 max=30646.9688 PROFFIT INFO: Inet/sig(Inet): min=-2.09 max=218.93 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 838 3442 5260 6358 6860 7992 8710 9126 9794 10240 10354 Percent 8.1 33.2 50.8 61.4 66.3 77.2 84.1 88.1 94.6 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5177 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 5177 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2033079- 133555 517 434025.89 78.29 100.00 133536- 4271 517 31567.00 20.30 100.00 4262- 2215 517 3032.34 7.37 98.26 2208- 1305 517 1690.81 3.99 54.16 1302- 876 517 1066.90 2.45 18.57 875- 578 517 714.59 1.77 7.93 577- 365 517 463.32 1.30 6.38 364- 169 517 265.02 0.77 1.16 168- 26 517 91.39 0.32 0.00 25- -1088 524 -121.47 -0.23 0.00 ------------------------------------------------------------------------------------ 2033079- -1088 5177 47215.49 11.62 38.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 517 117406.74 15.41 68.67 1.73- 1.26 517 92068.92 21.49 61.51 1.26- 1.09 517 63536.59 19.02 67.12 1.09- 0.97 517 57709.76 15.48 36.36 0.97- 0.88 517 15026.93 6.32 42.55 0.88- 0.81 517 56135.98 15.58 38.88 0.81- 0.76 517 19042.20 5.78 17.99 0.76- 0.71 517 22151.69 7.09 17.60 0.71- 0.67 517 25842.05 8.28 29.01 0.67- 0.63 524 3821.55 1.87 6.68 ------------------------------------------------------------------------------------ 6.00- 0.63 5177 47215.49 11.62 38.59 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:18:21 2019 Sorting 5177 observations 43 unique observations with > 7.00 F2/sig(F2) 5177 observations in 5 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 Total number of frames 516 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 12 frame = 1 scale 5177 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 Total number of frames 45 1271 observations > 7.00 F2/sig(F2) 1271 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 Total number of frames 45 Removing 'redundancy=1' reflections Average redundancy: 23.1 (Out of 1271 removed 3 = 1268, unique = 55) 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 1268 observations in 5 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 Total number of frames 45 55 unique data precomputed (should be 55) 55 unique data with 1268 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.1 (Out of 1268 removed 0 = 1268, unique = 55) 55 unique data precomputed (should be 55) 55 unique data with 1268 observations RMS deviation of equivalent data = 0.28581 Rint = 0.23408 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.23066, wR= 0.30813 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11149, wR= 0.16063, Acormin=0.515, Acormax=1.403, Acor_av=0.975 F test: Probability=1.000, F= 4.262 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09908, wR= 0.14488, Acormin=0.471, Acormax=1.464, Acor_av=0.937 F test: Probability=1.000, F= 1.263 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09760, wR= 0.15077, Acormin=0.533, Acormax=1.509, Acor_av=0.983 F test: Probability=0.667, F= 1.025 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08672, wR= 0.13094, Acormin=0.478, Acormax=1.629, Acor_av=0.950 F test: Probability=1.000, F= 1.296 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07883, wR= 0.12149, Acormin=0.536, Acormax=1.802, Acor_av=0.973 F test: Probability=0.999, F= 1.203 Final absorption model (ne=4, no=3): Rint= 0.07883, Acormin=0.536, Acormax=1.802, Acor_av=0.973 Combined refinement in use Rint: 0.23575 There are 45 active scales (one needs to be fixed) Refinement control: frame scale #41 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 68 pars with 2346 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.28581 Using Levenberg-Marquardt: 0.00010 New wR= 0.09853 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23408 with corrections 0.06371 Rint for all data: 0.23575 with corrections 0.06642 5 observations identified as outliers and rejected Cycle 2 wR= 0.07611 Using Levenberg-Marquardt: 0.00001 New wR= 0.07123 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.23071 with corrections 0.04934 Rint for all data: 0.23575 with corrections 0.05614 3 observations identified as outliers and rejected Cycle 3 wR= 0.06115 Using Levenberg-Marquardt: 0.00000 New wR= 0.05738 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22849 with corrections 0.04223 Rint for all data: 0.23575 with corrections 0.05103 0 observations identified as outliers and rejected Cycle 4 wR= 0.05738 Using Levenberg-Marquardt: 0.00000 New wR= 0.05654 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22849 with corrections 0.04189 Rint for all data: 0.23575 with corrections 0.05070 0 observations identified as outliers and rejected Cycle 5 wR= 0.05654 Using Levenberg-Marquardt: 0.00000 New wR= 0.05609 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.22849 with corrections 0.04174 Rint for all data: 0.23575 with corrections 0.05055 0 observations identified as outliers and rejected Final wR= 0.05609 Final frame scales: Min= 0.7627 Max= 1.2341 Final absorption correction factors: Amin= 0.4086 Amax= 1.6252 PROFFIT INFO: Inet (after scale3 abspack): min=-1137.0682 max=1332574.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=40.3568 max=25385.9492 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/104 5177 reflections read from tmp file 176 reflections are rejected (176 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 2 3 3 2 3 5 5 139 Initial Chi^2= 0.47476 Cycle 1, Chi^2= 1.02452 Current error model SIG(F2)^2 = 58.52*I_RAW + 10.80*I_BACK+(0.02919*)^2 Cycle 2, Chi^2= 1.01488 Current error model SIG(F2)^2 = 70.05*I_RAW + 8.26*I_BACK+(0.02531*)^2 Cycle 3, Chi^2= 1.00505 Current error model SIG(F2)^2 = 73.82*I_RAW + 7.62*I_BACK+(0.02458*)^2 Cycle 4, Chi^2= 1.00140 Current error model SIG(F2)^2 = 74.87*I_RAW + 7.45*I_BACK+(0.02445*)^2 Cycle 5, Chi^2= 1.00037 Current error model SIG(F2)^2 = 75.16*I_RAW + 7.41*I_BACK+(0.02442*)^2 Cycle 6, Chi^2= 1.00010 Current error model SIG(F2)^2 = 75.23*I_RAW + 7.40*I_BACK+(0.02441*)^2 Final Chi^2= 1.00010 Final error model SIG(F2)^2 = 75.23*I_RAW + 7.40*I_BACK+(0.02441*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1332574- 126070 517 407248.77 33.35 100.00 125655- 3641 517 31306.69 14.35 100.00 3637- 2170 517 2857.40 6.74 100.00 2169- 1225 517 1619.64 4.31 76.40 1224- 824 517 1011.48 3.01 36.56 824- 552 517 687.44 2.60 21.47 551- 356 517 449.43 2.09 10.64 355- 166 517 260.32 1.53 4.45 166- 26 517 91.30 0.77 0.58 26- -1137 524 -119.17 -0.48 0.00 ------------------------------------------------------------------------------------ 1332574- -1137 5177 44480.94 6.82 44.95 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 517 111586.40 11.04 73.11 1.73- 1.26 517 86449.25 10.53 65.96 1.26- 1.09 517 60587.34 8.90 73.69 1.09- 0.97 517 53398.72 7.29 39.85 0.97- 0.88 517 12965.23 4.72 54.74 0.88- 0.81 517 54574.90 8.66 49.13 0.81- 0.76 517 17761.10 4.03 22.44 0.76- 0.71 517 20389.23 5.24 25.15 0.71- 0.67 517 23956.10 5.93 35.59 0.67- 0.63 524 3693.40 1.88 10.31 ------------------------------------------------------------------------------------ 6.00- 0.63 5177 44480.94 6.82 44.95 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 517 111586.40 11.04 73.11 6.00- 1.26 1034 99017.82 10.79 69.54 6.00- 1.09 1551 86207.66 10.16 70.92 6.00- 0.97 2068 78005.43 9.44 63.15 6.00- 0.88 2585 64997.39 8.50 61.47 6.00- 0.81 3102 63260.31 8.53 59.41 6.00- 0.76 3619 56760.42 7.88 54.13 6.00- 0.71 4136 52214.02 7.55 50.51 6.00- 0.67 4653 49074.25 7.37 48.85 6.00- 0.63 5177 44480.94 6.82 44.95 ------------------------------------------------------------------------------------ 6.00- 0.63 5177 44480.94 6.82 44.95 Scale applied to data: s=0.750427 (maximum obs:1332574.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.051; Rsigma 0.035: data 5177 -> merged 162 With outlier rejection... Rint 0.044; Rsigma 0.035: data 5161 -> merged 162 Rejected total: 16, method kkm 9, method Blessing 7 Completeness direct cell (a, b, c) = (10.420, 10.420, 10.420), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627233, 6.016208 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.43 - 1.76 14 14 33.86 100.00 474 1.74 - 1.27 14 14 37.57 100.00 526 1.26 - 1.06 14 14 42.07 100.00 589 1.05 - 0.97 14 14 36.43 100.00 510 0.95 - 0.88 14 14 37.79 100.00 529 0.87 - 0.81 14 14 33.86 100.00 474 0.80 - 0.76 14 14 35.36 100.00 495 0.76 - 0.72 14 14 29.64 100.00 415 0.72 - 0.69 14 14 32.43 100.00 454 0.69 - 0.65 19 19 27.26 100.00 518 --------------------------------------------------------------- 10.43 - 0.65 145 145 34.37 100.00 4984 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:18:21 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.414817 10.430843 10.415300 89.9898 89.9692 89.9991 5152 Reflections read from file xs2212a.hkl 5122 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.52 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2574 0 3398 3395 5122 N (int>3sigma) = 0 0 0 0 1207 0 1568 1553 2246 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.7 30.5 31.7 Mean int/sigma = 0.0 0.0 0.0 0.0 4.2 0.0 6.7 6.5 6.5 Lattice type: F chosen Volume: 1131.47 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.363 7.367 7.370 60.02 60.04 90.00 Niggli form: a.a = 54.208 b.b = 54.266 c.c = 54.311 b.c = 27.129 a.c = 27.101 a.b = 0.003 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.170 CUBIC F-lattice R(int) = 0.049 [ 4891] Vol = 1131.5 Cell: 10.415 10.415 10.431 90.00 90.01 90.03 Volume: 1131.47 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.121 TETRAGONAL I-lattice R(int) = 0.047 [ 4506] Vol = 565.7 Cell: 7.370 7.370 10.415 90.01 89.97 89.91 Volume: 565.73 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.064 TETRAGONAL I-lattice R(int) = 0.049 [ 4505] Vol = 565.7 Cell: 7.363 7.367 10.431 89.99 89.99 90.00 Volume: 565.73 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.064 ORTHORHOMBIC F-lattice R(int) = 0.047 [ 4452] Vol = 1131.5 Cell: 10.415 10.415 10.431 90.00 90.01 89.97 Volume: 1131.47 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.136 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4432] Vol = 565.7 Cell: 10.415 7.370 7.370 89.91 89.97 90.01 Volume: 565.73 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.006 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 4435] Vol = 565.7 Cell: 7.363 7.367 10.431 90.01 90.01 90.00 Volume: 565.73 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.062 MONOCLINIC I-lattice R(int) = 0.045 [ 3908] Vol = 565.7 Cell: 7.370 10.415 7.371 90.02 90.09 90.02 Volume: 565.73 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.060 MONOCLINIC I-lattice R(int) = 0.045 [ 3912] Vol = 565.7 Cell: 7.370 10.415 7.370 90.03 90.09 90.01 Volume: 565.73 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.004 MONOCLINIC I-lattice R(int) = 0.043 [ 3890] Vol = 565.7 Cell: 7.367 7.363 10.431 89.99 90.01 90.00 Volume: 565.73 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.005 MONOCLINIC I-lattice R(int) = 0.043 [ 3905] Vol = 565.7 Cell: 7.363 7.367 10.431 89.99 90.01 90.00 Volume: 565.73 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.038 [ 2862] Vol = 282.9 Cell: 7.363 7.367 7.370 60.02 60.04 90.00 Volume: 282.87 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -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 2574 0 3406 3395 5122 N (int>3sigma) = 0 0 0 0 1207 0 1581 1553 2246 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.1 30.5 31.7 Mean int/sigma = 0.0 0.0 0.0 0.0 4.2 0.0 6.6 6.5 6.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.113 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 37 37 380 1007 N I>3s 2 2 2 562 0.0 0.0 0.0 1.9 0.9 0.9 0.3 5.3 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 0.049 4539 Fd-3m 1 1 227 C N N N N 37 2284 0.049 4601 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415300 10.414817 10.430843 89.9991 90.0102 90.0308 ZERR 5.00 0.001211 0.001489 0.001644 0.0122 0.0111 0.0106 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1227799- 98121 629 621 27 23.0 355765.76 31.51 0.041 0.049 82418- 1932 978 974 27 36.1 5542.43 9.08 0.075 0.081 1801- 821 1027 1025 27 38.0 1207.50 3.29 0.208 0.282 818- 347 1031 1030 27 38.1 535.67 2.17 0.350 0.494 346- 68 766 765 27 28.3 230.12 1.21 0.583 0.886 65- -163 746 746 27 27.6 10.98 0.21 0.963 3.667 ------------------------------------------------------------------------------------------- 1227799- -163 5177 5161 162 31.9 44236.10 6.80 0.044 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-1.27 1002 998 27 37.0 101317.58 11.05 0.038 0.043 0.027 1.26-0.97 1103 1099 28 39.3 53258.43 7.66 0.039 0.047 0.032 0.95-0.81 948 946 27 35.0 36805.71 7.16 0.049 0.063 0.039 0.81-0.73 922 922 27 34.1 14555.94 3.85 0.062 0.080 0.055 0.73-0.67 812 810 28 28.9 23088.55 5.62 0.067 0.087 0.054 0.66-0.63 390 386 25 15.4 4445.75 2.03 0.094 0.069 0.113 ------------------------------------------------------------------------------------------------------ inf-0.63 5177 5161 162 31.9 44236.10 6.80 0.044 0.053 0.035 inf-0.65 4995 4982 144 34.6 45585.42 6.96 0.044 0.052 0.034 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-1.27 998 27 27 100.0 37.0 101317.58 65.17 0.038 0.006 1.26-0.97 1099 28 28 100.0 39.3 53258.43 45.43 0.039 0.006 0.95-0.81 946 27 27 100.0 35.0 36805.71 43.09 0.049 0.008 0.81-0.73 922 27 27 100.0 34.1 14555.94 20.54 0.062 0.011 0.73-0.67 810 28 28 100.0 28.9 23088.55 31.85 0.067 0.010 0.66-0.63 386 25 25 100.0 15.4 4445.75 8.04 0.094 0.030 -------------------------------------------------------------------------------------------- inf-0.63 5161 162 162 100.0 31.9 44236.10 39.44 0.044 0.008 inf-0.65 4982 144 144 100.0 34.6 45585.42 40.63 0.044 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:24:14 2019) ID: 3668; threads 40; handles 809; mem 514772.00 (1204692.00)kB; time: 1w 5d 0h 35m 2s MEMORY INFO: Memory PF:226.0, Ph:557.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:502.7,peak PF: 700.2, WS: 471.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:227.0, Ph:559.0, V:1178.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:504.5,peak PF: 700.2, WS: 473.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:24:14 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000014 0.000014 ) -0.003867 -0.014380 0.066544 ( 0.000015 0.000017 0.000016 ) 10.42433 ( 0.00234 ) 10.43788 ( 0.00219 ) 10.40727 ( 0.00243 ) 89.88512 ( 0.01805 ) 89.79539 ( 0.01858 ) 90.20497 ( 0.01792 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:24:14 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000017 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000014 0.000014 ) -0.003867 -0.014380 0.066544 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004633 0.000003 -0.000009 ( 0.000002 0.000001 0.000001 ) 0.000003 0.004619 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000004 0.004649 ( 0.000001 0.000001 0.000002 ) unit cell: 10.424(2) 10.438(2) 10.407(2) 89.885(18) 89.795(19) 90.205(18) V = 1132.4(4) unit cell: 10.4198(8) 10.4198(8) 10.4198(8) 90.0 90.0 90.0 V = 1131.29(15) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 219 peaks identified as outliers and rejected 219 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 219 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 219 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.906 ( 0.080) | 0.934 ( 0.165) | 0.922 ( 0.398) | 1.00- 0.88 | 22 | 0.960 ( 0.074) | 1.004 ( 0.125) | 1.180 ( 0.494) | 0.88- 0.79 | 22 | 0.984 ( 0.058) | 1.025 ( 0.139) | 1.235 ( 0.386) | 0.79- 0.70 | 22 | 0.979 ( 0.045) | 0.955 ( 0.108) | 1.275 ( 0.476) | 0.69- 0.63 | 21 | 0.945 ( 0.037) | 0.919 ( 0.082) | 1.330 ( 0.484) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 219 | 0.932 ( 0.193) | 0.942 ( 0.158) | 1.114 ( 0.916) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.87 | 25 | 0.945 ( 0.067) | 0.936 ( 0.094) | 1.074 ( 0.403) | 0.86- 0.73 | 25 | 0.958 ( 0.050) | 0.919 ( 0.091) | 1.335 ( 0.450) | 0.73- 0.63 | 29 | 0.929 ( 0.037) | 0.880 ( 0.095) | 1.340 ( 0.463) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 254 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.061 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 277 peaks identified as outliers and rejected 277 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 277 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 277 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.910 ( 0.121) | 0.992 ( 0.359) | 0.985 ( 0.566) | 1.75- 1.56 | 28 | 0.959 ( 0.113) | 0.971 ( 0.143) | 0.999 ( 0.439) | 1.56- 1.35 | 28 | 0.959 ( 0.097) | 0.971 ( 0.157) | 0.802 ( 0.335) | 1.35- 1.19 | 28 | 0.939 ( 0.098) | 0.977 ( 0.159) | 0.717 ( 0.268) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.016 ( 0.108) | 0.880 ( 0.347) | 1.06- 0.91 | 28 | 1.003 ( 0.076) | 1.052 ( 0.122) | 0.969 ( 0.382) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 0.999 ( 0.122) | 1.085 ( 0.341) | 0.86- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.132) | 1.179 ( 0.466) | 0.73- 0.63 | 25 | 1.004 ( 0.041) | 1.024 ( 0.127) | 1.077 ( 0.358) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 277 | 0.969 ( 0.097) | 0.992 ( 0.175) | 0.955 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 276 obs out of 277 (total:277,skipped:0) (99.64%) UB - matrix: 0.066020 0.015435 0.006402 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000023 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000002 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000002 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.996(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 276 1 1 1 OTKP changes: 276 1 1 1 OTKP changes: 276 1 1 1 No constraint UB - matrix: 0.065951 0.015338 0.006295 ( 0.000017 0.000012 0.000013 ) -0.016327 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002849 -0.014645 0.066457 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065951 0.015338 0.006295 ( 0.000017 0.000012 0.000013 ) -0.016327 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002849 -0.014645 0.066457 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 276 obs out of 277 (total:277,skipped:0) (99.64%) unit cell: 10.431(2) 10.410(2) 10.4178(19) 89.888(16) 90.087(17) 89.951(18) V = 1131.2(4) unit cell: 10.4194(6) 10.4194(6) 10.4194(6) 90.0 90.0 90.0 V = 1131.17(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065951 0.015338 0.006295 ( 0.000017 0.000012 0.000013 ) -0.016327 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002849 -0.014645 0.066457 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065951 0.015338 0.006295 ( 0.000017 0.000012 0.000013 ) -0.016327 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002849 -0.014645 0.066457 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 276 obs out of 277 (total:277,skipped:0) (99.64%) unit cell: 10.431(2) 10.410(2) 10.4178(19) 89.888(16) 90.087(17) 89.951(18) V = 1131.2(4) unit cell: 10.4194(6) 10.4194(6) 10.4194(6) 90.0 90.0 90.0 V = 1131.17(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 276 obs out of 277 (total:277,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 272 peaks identified as outliers and rejected 272 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 272 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 272 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.57 | 27 | 0.974 ( 0.112) | 0.999 ( 0.142) | 1.003 ( 0.428) | 1.50- 1.35 | 27 | 0.963 ( 0.092) | 0.979 ( 0.160) | 0.818 ( 0.386) | 1.35- 1.19 | 27 | 0.940 ( 0.103) | 0.968 ( 0.154) | 0.731 ( 0.285) | 1.19- 1.06 | 27 | 0.978 ( 0.066) | 1.024 ( 0.101) | 0.888 ( 0.347) | 1.06- 0.92 | 27 | 1.010 ( 0.075) | 1.070 ( 0.119) | 0.971 ( 0.376) | 0.92- 0.87 | 27 | 1.005 ( 0.061) | 0.992 ( 0.113) | 1.132 ( 0.382) | 0.87- 0.73 | 27 | 1.043 ( 0.052) | 1.032 ( 0.132) | 1.207 ( 0.467) | 0.73- 0.63 | 29 | 1.001 ( 0.040) | 1.013 ( 0.122) | 1.092 ( 0.393) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 272 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.965 ( 0.413) | 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_6_1.rpb PROFFITPEAK info: 71 peaks in the peak location table UB fit with 19 obs out of 45 (total:45,skipped:0) (42.22%) UB - matrix: 0.066153 0.014618 0.006143 ( 0.000112 0.000420 0.000139 ) -0.016298 0.065421 0.013117 ( 0.000131 0.000490 0.000162 ) -0.003707 -0.014725 0.066515 ( 0.000144 0.000538 0.000178 ) M - matrix: 0.004656 -0.000045 -0.000054 ( 0.000015 0.000030 0.000014 ) -0.000045 0.004710 -0.000032 ( 0.000030 0.000067 0.000038 ) -0.000054 -0.000032 0.004634 ( 0.000014 0.000038 0.000024 ) unit cell: 10.40(3) 10.34(7) 10.42(3) 89.6(4) 89.3(2) 89.4(4) V = 1120(9) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table UB fit with 19 obs out of 45 (total:45,skipped:0) (42.22%) UB - matrix: 0.066153 0.014618 0.006143 ( 0.000112 0.000420 0.000139 ) -0.016298 0.065421 0.013117 ( 0.000131 0.000490 0.000162 ) -0.003707 -0.014725 0.066515 ( 0.000144 0.000538 0.000178 ) M - matrix: 0.004656 -0.000045 -0.000054 ( 0.000015 0.000030 0.000014 ) -0.000045 0.004710 -0.000032 ( 0.000030 0.000067 0.000038 ) -0.000054 -0.000032 0.004634 ( 0.000014 0.000038 0.000024 ) unit cell: 10.40(3) 10.34(7) 10.42(3) 89.6(4) 89.3(2) 89.4(4) V = 1120(9) OTKP changes: 14 1 1 1 OTKP changes: 14 1 1 1 No constraint UB - matrix: 0.066097 0.015375 0.006112 ( 0.000080 0.000187 0.000086 ) -0.016455 0.064774 0.012832 ( 0.000088 0.000206 0.000095 ) -0.002925 -0.013932 0.066408 ( 0.000067 0.000156 0.000072 ) M - matrix: 0.004648 -0.000009 -0.000001 ( 0.000011 0.000014 0.000007 ) -0.000009 0.004626 -0.000000 ( 0.000014 0.000028 0.000013 ) -0.000001 -0.000000 0.004612 ( 0.000007 0.000013 0.000010 ) Constraint UB - matrix: 0.066097 0.015375 0.006112 ( 0.000080 0.000187 0.000086 ) -0.016455 0.064774 0.012832 ( 0.000088 0.000206 0.000095 ) -0.002925 -0.013932 0.066408 ( 0.000067 0.000156 0.000072 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000003 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000003 ) UB fit with 40 obs out of 45 (total:45,skipped:0) (88.89%) unit cell: 10.404(15) 10.43(3) 10.444(13) 90.00(15) 89.98(11) 89.89(17) V = 1133(4) unit cell: 10.426(3) 10.426(3) 10.426(3) 90.0 90.0 90.0 V = 1133.2(7) UB fit with 40 obs out of 45 (total:45,skipped:0) (88.89%) UB - matrix: 0.066097 0.015375 0.006111 ( 0.000080 0.000187 0.000086 ) -0.016457 0.064777 0.012831 ( 0.000088 0.000206 0.000095 ) -0.002921 -0.013938 0.066410 ( 0.000067 0.000156 0.000072 ) M - matrix: 0.004648 -0.000009 -0.000001 ( 0.000011 0.000014 0.000007 ) -0.000009 0.004627 -0.000001 ( 0.000014 0.000028 0.000012 ) -0.000001 -0.000001 0.004612 ( 0.000007 0.000012 0.000010 ) unit cell: 10.404(15) 10.43(3) 10.444(13) 89.99(15) 89.98(11) 89.89(17) V = 1133(4) OTKP changes: 19 1 1 1 OTKP changes: 19 1 1 1 No constraint UB - matrix: 0.066086 0.015269 0.006217 ( 0.000065 0.000152 0.000070 ) -0.016571 0.064877 0.012726 ( 0.000086 0.000203 0.000093 ) -0.003022 -0.014089 0.066640 ( 0.000044 0.000103 0.000047 ) M - matrix: 0.004651 -0.000023 -0.000001 ( 0.000009 0.000012 0.000006 ) -0.000023 0.004641 -0.000018 ( 0.000012 0.000027 0.000010 ) -0.000001 -0.000018 0.004642 ( 0.000006 0.000010 0.000007 ) Constraint UB - matrix: 0.066086 0.015269 0.006217 ( 0.000065 0.000152 0.000070 ) -0.016571 0.064877 0.012726 ( 0.000086 0.000203 0.000093 ) -0.003022 -0.014089 0.066640 ( 0.000044 0.000103 0.000047 ) M - matrix: 0.004636 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.004636 0.000000 ( 0.000000 0.000003 0.000000 ) 0.000000 0.000000 0.004636 ( 0.000000 0.000000 0.000003 ) UB fit with 40 obs out of 45 (total:45,skipped:0) (88.89%) unit cell: 10.401(12) 10.41(3) 10.411(9) 89.77(12) 89.98(8) 89.71(15) V = 1127(4) unit cell: 10.408(4) 10.408(4) 10.408(4) 90.0 90.0 90.0 V = 1127.5(7) 45 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Run 6 Omega scan: (-99.000 - -74.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 474 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 40 obs out of 45 (total:45,skipped:0) (88.89%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_1.rpb 0 of 40 peaks identified as outliers and rejected 40 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 40 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 40 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.15- 3.11 | 4 | 0.881 ( 0.174) | 0.856 ( 0.237) | 0.767 ( 0.267) | 2.12- 1.76 | 4 | 0.857 ( 0.106) | 0.894 ( 0.164) | 0.588 ( 0.142) | 1.75- 1.58 | 4 | 0.779 ( 0.061) | 0.760 ( 0.119) | 0.843 ( 0.422) | 1.46- 1.36 | 4 | 0.970 ( 0.060) | 1.017 ( 0.061) | 0.939 ( 0.134) | 1.30- 1.16 | 4 | 0.962 ( 0.092) | 0.959 ( 0.177) | 0.842 ( 0.136) | 1.06- 0.92 | 4 | 1.003 ( 0.065) | 1.037 ( 0.123) | 1.078 ( 0.231) | 0.88- 0.82 | 4 | 1.004 ( 0.047) | 1.027 ( 0.152) | 0.966 ( 0.163) | 0.79- 0.73 | 4 | 0.984 ( 0.046) | 0.942 ( 0.089) | 1.254 ( 0.447) | 0.72- 0.68 | 4 | 0.979 ( 0.014) | 0.871 ( 0.041) | 1.300 ( 0.649) | 0.68- 0.63 | 4 | 0.906 ( 0.027) | 0.836 ( 0.034) | 1.325 ( 0.299) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.15- 0.63 | 40 | 0.933 ( 0.108) | 0.920 ( 0.160) | 0.990 ( 0.405) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 40 obs out of 40 (total:40,skipped:0) (100.00%) UB - matrix: 0.065956 0.015554 0.006289 ( 0.000044 0.000102 0.000050 ) -0.016449 0.064864 0.012848 ( 0.000051 0.000119 0.000058 ) -0.002907 -0.013995 0.066557 ( 0.000038 0.000089 0.000044 ) M - matrix: 0.004629 -0.000000 0.000010 ( 0.000006 0.000008 0.000004 ) -0.000000 0.004645 -0.000000 ( 0.000008 0.000016 0.000007 ) 0.000010 -0.000000 0.004634 ( 0.000004 0.000007 0.000006 ) unit cell: 10.425(8) 10.407(17) 10.419(7) 90.00(9) 90.12(6) 90.00(10) V = 1130(2) OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 No constraint UB - matrix: 0.066050 0.015568 0.006257 ( 0.000032 0.000073 0.000036 ) -0.016445 0.064819 0.012821 ( 0.000047 0.000109 0.000053 ) -0.003014 -0.014056 0.066620 ( 0.000028 0.000065 0.000032 ) M - matrix: 0.004642 0.000005 0.000002 ( 0.000004 0.000006 0.000003 ) 0.000005 0.004641 -0.000008 ( 0.000006 0.000014 0.000006 ) 0.000002 -0.000008 0.004642 ( 0.000003 0.000006 0.000004 ) Constraint UB - matrix: 0.066050 0.015568 0.006257 ( 0.000032 0.000073 0.000036 ) -0.016445 0.064819 0.012821 ( 0.000047 0.000109 0.000053 ) -0.003014 -0.014056 0.066620 ( 0.000028 0.000065 0.000032 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 40 obs out of 40 (total:40,skipped:0) (100.00%) unit cell: 10.410(6) 10.411(15) 10.411(6) 89.90(7) 90.02(4) 90.06(7) V = 1128(2) unit cell: 10.4109(15) 10.4109(15) 10.4109(15) 90.0 90.0 90.0 V = 1128.4(3) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - -74.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 477 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 40 obs out of 40 (total:40,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_1.rpb 0 of 38 peaks identified as outliers and rejected 38 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 38 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 38 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 3.12 | 4 | 0.883 ( 0.175) | 0.857 ( 0.237) | 0.911 ( 0.045) | 2.12- 1.76 | 4 | 0.824 ( 0.105) | 0.851 ( 0.171) | 0.587 ( 0.095) | 1.75- 1.45 | 4 | 0.801 ( 0.074) | 0.798 ( 0.137) | 0.921 ( 0.361) | 1.36- 1.30 | 4 | 0.964 ( 0.062) | 0.971 ( 0.132) | 0.814 ( 0.111) | 1.30- 1.06 | 4 | 0.999 ( 0.073) | 1.023 ( 0.125) | 1.051 ( 0.244) | 1.00- 0.88 | 4 | 1.008 ( 0.066) | 1.042 ( 0.121) | 0.913 ( 0.079) | 0.88- 0.79 | 4 | 0.998 ( 0.045) | 1.018 ( 0.153) | 0.965 ( 0.165) | 0.78- 0.72 | 4 | 0.973 ( 0.045) | 0.892 ( 0.088) | 1.652 ( 0.550) | 0.69- 0.68 | 4 | 0.977 ( 0.018) | 0.877 ( 0.035) | 0.924 ( 0.208) | 0.67- 0.67 | 2 | 0.886 ( 0.015) | 0.849 ( 0.044) | 1.492 ( 0.173) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 0.67 | 38 | 0.934 ( 0.111) | 0.921 ( 0.163) | 0.998 ( 0.382) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.0 | 124 | 0.989 ( 0.040) | 1.033 ( 0.067) | 1.119 ( 0.478) | 10.1-14.6 | 124 | 0.993 ( 0.046) | 1.048 ( 0.069) | 1.109 ( 0.536) | 14.6-18.8 | 124 | 0.996 ( 0.191) | 1.034 ( 0.101) | 1.132 ( 1.002) | 18.8-23.4 | 124 | 0.969 ( 0.062) | 1.015 ( 0.083) | 0.924 ( 0.421) | 23.4-27.0 | 124 | 0.969 ( 0.063) | 1.000 ( 0.096) | 0.990 ( 0.439) | 27.0-32.1 | 124 | 0.946 ( 0.080) | 0.963 ( 0.104) | 0.954 ( 0.458) | 32.1-36.2 | 124 | 0.927 ( 0.154) | 0.922 ( 0.141) | 1.060 ( 0.670) | 36.2-38.9 | 124 | 0.879 ( 0.104) | 0.871 ( 0.256) | 1.023 ( 0.471) | 38.9-41.9 | 124 | 0.908 ( 0.093) | 0.858 ( 0.127) | 1.035 ( 0.473) | 41.9-50.1 | 128 | 0.863 ( 0.123) | 0.795 ( 0.142) | 0.929 ( 0.438) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1244 | 0.944 ( 0.116) | 0.953 ( 0.155) | 1.027 ( 0.569) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.14 e2 dimension: a=-0.0068 b=1.24 e3 dimension: a=0.0007 b=1.09 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 4496 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 14:24:32 2019 PROFFITMAIN - Started at Wed Aug 21 14:24:32 2019 OTKP changes: 973 2 5 6 OTKP changes: 973 2 5 6 OTKP changes: 973 2 5 6 No constraint UB - matrix: 0.066059 0.015017 0.006752 ( 0.000014 0.000016 0.000015 ) -0.016058 0.064717 0.013107 ( 0.000013 0.000015 0.000014 ) -0.003765 -0.014355 0.066590 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004636 0.000007 -0.000015 ( 0.000002 0.000001 0.000001 ) 0.000007 0.004620 -0.000006 ( 0.000001 0.000002 0.000002 ) -0.000015 -0.000006 0.004652 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: 0.066059 0.015017 0.006752 ( 0.000014 0.000016 0.000015 ) -0.016058 0.064717 0.013107 ( 0.000013 0.000015 0.000014 ) -0.003765 -0.014355 0.066590 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004636 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004636 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004636 ( 0.000000 0.000000 0.000001 ) UB fit with 985 obs out of 1244 (total:1244,skipped:0) (79.18%) unit cell: 10.418(2) 10.436(2) 10.400(2) 89.923(19) 89.813(18) 90.084(17) V = 1130.6(4) unit cell: 10.4177(8) 10.4177(8) 10.4177(8) 90.0 90.0 90.0 V = 1130.62(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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 186 obs out of 219 (total:219,skipped:0) (84.93%) UB - matrix: 0.066503 0.011701 0.008959 ( 0.000032 0.000043 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000031 0.000041 0.000034 ) -0.006051 -0.013931 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004647 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.60(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066501 0.011703 0.008957 ( 0.000032 0.000042 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006047 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004647 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066501 0.011703 0.008957 ( 0.000032 0.000042 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006047 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000002 ) UB fit with 188 obs out of 219 (total:219,skipped:0) (85.84%) unit cell: 10.405(5) 10.502(6) 10.456(6) 90.61(5) 90.19(4) 89.64(4) V = 1143(1) unit cell: 10.4541(19) 10.4541(19) 10.4541(19) 90.0 90.0 90.0 V = 1142.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 202 obs out of 219 (total:219,skipped:0) (92.24%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068147 -0.000275 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000058 0.067610 0.000629 ( 0.000031 0.000040 0.000032 ) -0.000035 -0.000063 0.067944 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004644 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004571 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068147 -0.000275 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000058 0.067610 0.000629 ( 0.000031 0.000040 0.000032 ) -0.000035 -0.000063 0.067944 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 205 obs out of 219 (total:219,skipped:0) (93.61%) unit cell: 10.408(4) 10.491(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1139.9(9) unit cell: 10.4462(13) 10.4462(13) 10.4462(13) 90.0 90.0 90.0 V = 1139.9(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.066336 0.014186 0.006779 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064704 0.012861 ( 0.000017 0.000022 0.000023 ) -0.004076 -0.014197 0.066901 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.393(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4047(5) 10.4047(5) 10.4047(5) 90.0 90.0 90.0 V = 1126.40(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065861 0.015182 0.006790 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064744 0.013256 ( 0.000016 0.000011 0.000016 ) -0.003655 -0.014499 0.066475 ( 0.000021 0.000014 0.000020 ) M - matrix: 0.004609 0.000012 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000012 0.004633 -0.000002 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000002 0.004641 ( 0.000002 0.000001 0.000003 ) unit cell: 10.448(3) 10.4213(19) 10.412(3) 89.969(19) 89.89(2) 90.155(18) V = 1133.6(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065848 0.015171 0.006798 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064760 0.013256 ( 0.000016 0.000011 0.000016 ) -0.003662 -0.014466 0.066474 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004608 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004633 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004641 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065848 0.015171 0.006798 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064760 0.013256 ( 0.000016 0.000011 0.000016 ) -0.003662 -0.014466 0.066474 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.449(3) 10.4205(19) 10.412(3) 90.000(18) 89.89(2) 90.140(18) V = 1133.8(5) unit cell: 10.4273(5) 10.4273(5) 10.4273(5) 90.0 90.0 90.0 V = 1133.75(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.144) HKL list info: 1274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065848 0.015171 0.006798 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064760 0.013256 ( 0.000016 0.000011 0.000016 ) -0.003662 -0.014466 0.066474 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004608 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004633 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004641 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065848 0.015171 0.006798 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064760 0.013256 ( 0.000016 0.000011 0.000016 ) -0.003662 -0.014466 0.066474 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.449(3) 10.4205(19) 10.412(3) 90.000(18) 89.89(2) 90.140(18) V = 1133.8(5) unit cell: 10.4273(5) 10.4273(5) 10.4273(5) 90.0 90.0 90.0 V = 1133.75(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065848 0.015171 0.006798 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064760 0.013256 ( 0.000016 0.000011 0.000016 ) -0.003662 -0.014466 0.066474 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004608 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004633 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004641 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065848 0.015171 0.006798 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064760 0.013256 ( 0.000016 0.000011 0.000016 ) -0.003662 -0.014466 0.066474 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.449(3) 10.4205(19) 10.412(3) 90.000(18) 89.89(2) 90.140(18) V = 1133.8(5) unit cell: 10.4273(5) 10.4273(5) 10.4273(5) 90.0 90.0 90.0 V = 1133.75(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066087 0.015228 0.006576 ( 0.000014 0.000019 0.000016 ) -0.016353 0.064715 0.012940 ( 0.000012 0.000016 0.000013 ) -0.003376 -0.014187 0.066484 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004646 -0.000004 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004621 -0.000006 ( 0.000001 0.000002 0.000001 ) -0.000001 -0.000006 0.004631 ( 0.000001 0.000001 0.000002 ) unit cell: 10.406(2) 10.434(2) 10.4232(18) 89.929(16) 89.982(16) 89.950(18) V = 1131.7(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066068 0.015211 0.006546 ( 0.000013 0.000018 0.000015 ) -0.016320 0.064702 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003367 -0.014171 0.066512 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004643 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004619 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004635 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066068 0.015211 0.006546 ( 0.000013 0.000018 0.000015 ) -0.016320 0.064702 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003367 -0.014171 0.066512 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.410(2) 10.437(2) 10.4188(18) 89.947(16) 89.963(16) 89.959(18) V = 1132.0(4) unit cell: 10.4219(5) 10.4219(5) 10.4219(5) 90.0 90.0 90.0 V = 1132.00(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.144) HKL list info: 1300 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066068 0.015211 0.006546 ( 0.000013 0.000018 0.000015 ) -0.016320 0.064702 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003367 -0.014171 0.066512 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004643 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004619 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004635 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066068 0.015211 0.006546 ( 0.000013 0.000018 0.000015 ) -0.016320 0.064702 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003367 -0.014171 0.066512 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.410(2) 10.437(2) 10.4188(18) 89.947(16) 89.963(16) 89.959(18) V = 1132.0(4) unit cell: 10.4219(5) 10.4219(5) 10.4219(5) 90.0 90.0 90.0 V = 1132.00(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068122 -0.000046 -0.000033 ( 0.000011 0.000015 0.000012 ) 0.000002 0.067975 -0.000049 ( 0.000013 0.000018 0.000015 ) 0.000007 0.000008 0.068080 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004641 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004621 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004635 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068122 -0.000046 -0.000033 ( 0.000011 0.000015 0.000012 ) 0.000002 0.067975 -0.000049 ( 0.000013 0.000018 0.000015 ) 0.000007 0.000008 0.068080 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.4122(17) 10.435(3) 10.4187(15) 89.965(16) 89.978(13) 89.963(17) V = 1132.0(4) unit cell: 10.4219(5) 10.4219(5) 10.4219(5) 90.0 90.0 90.0 V = 1131.98(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 250 obs out of 272 (total:272,skipped:0) (91.91%) UB - matrix: 0.065949 0.015334 0.006318 ( 0.000017 0.000013 0.000013 ) -0.016328 0.064766 0.013396 ( 0.000022 0.000016 0.000017 ) -0.003162 -0.014525 0.066453 ( 0.000032 0.000024 0.000024 ) M - matrix: 0.004626 -0.000000 -0.000012 ( 0.000002 0.000002 0.000002 ) -0.000000 0.004641 -0.000001 ( 0.000002 0.000002 0.000002 ) -0.000012 -0.000001 0.004635 ( 0.000002 0.000002 0.000003 ) unit cell: 10.429(3) 10.412(3) 10.418(4) 89.99(2) 89.85(3) 90.00(2) V = 1131.2(6) OTKP changes: 271 1 1 1 OTKP changes: 271 1 1 1 OTKP changes: 271 1 1 1 No constraint UB - matrix: 0.065960 0.015345 0.006299 ( 0.000016 0.000012 0.000013 ) -0.016343 0.064754 0.013396 ( 0.000018 0.000013 0.000014 ) -0.002852 -0.014640 0.066464 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004626 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004637 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065960 0.015345 0.006299 ( 0.000016 0.000012 0.000013 ) -0.016343 0.064754 0.013396 ( 0.000018 0.000013 0.000014 ) -0.002852 -0.014640 0.066464 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 271 obs out of 272 (total:272,skipped:0) (99.63%) unit cell: 10.429(2) 10.410(2) 10.4167(19) 89.890(16) 90.087(17) 89.946(18) V = 1130.8(4) unit cell: 10.4184(6) 10.4184(6) 10.4184(6) 90.0 90.0 90.0 V = 1130.84(11) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.144) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065960 0.015345 0.006299 ( 0.000016 0.000012 0.000013 ) -0.016343 0.064754 0.013396 ( 0.000018 0.000013 0.000014 ) -0.002852 -0.014640 0.066464 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004626 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004637 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065960 0.015345 0.006299 ( 0.000016 0.000012 0.000013 ) -0.016343 0.064754 0.013396 ( 0.000018 0.000013 0.000014 ) -0.002852 -0.014640 0.066464 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 271 obs out of 272 (total:272,skipped:0) (99.63%) unit cell: 10.429(2) 10.410(2) 10.4167(19) 89.890(16) 90.087(17) 89.946(18) V = 1130.8(4) unit cell: 10.4184(6) 10.4184(6) 10.4184(6) 90.0 90.0 90.0 V = 1130.84(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 271 obs out of 272 (total:272,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068028 -0.000091 0.000067 ( 0.000017 0.000013 0.000013 ) 0.000054 0.068106 -0.000088 ( 0.000014 0.000010 0.000011 ) -0.000014 0.000008 0.068084 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.004628 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004639 -0.000005 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000005 0.004635 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068028 -0.000091 0.000067 ( 0.000017 0.000013 0.000013 ) 0.000054 0.068106 -0.000088 ( 0.000014 0.000010 0.000011 ) -0.000014 0.000008 0.068084 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 271 obs out of 272 (total:272,skipped:0) (99.63%) unit cell: 10.427(3) 10.4146(16) 10.4181(19) 89.932(13) 90.045(17) 89.970(16) V = 1131.3(4) unit cell: 10.4198(6) 10.4198(6) 10.4198(6) 90.0 90.0 90.0 V = 1131.29(11) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 38 obs out of 38 (total:38,skipped:0) (100.00%) UB - matrix: 0.066054 0.015575 0.006260 ( 0.000030 0.000072 0.000037 ) -0.016440 0.064770 0.012865 ( 0.000043 0.000101 0.000052 ) -0.003020 -0.014004 0.066599 ( 0.000027 0.000064 0.000033 ) M - matrix: 0.004642 0.000006 0.000001 ( 0.000004 0.000006 0.000003 ) 0.000006 0.004634 -0.000002 ( 0.000006 0.000013 0.000006 ) 0.000001 -0.000002 0.004640 ( 0.000003 0.000006 0.000005 ) unit cell: 10.410(6) 10.420(14) 10.413(6) 89.98(7) 90.01(4) 90.08(7) V = 1129(2) OTKP changes: 38 1 1 1 OTKP changes: 38 1 1 1 OTKP changes: 38 1 1 1 OTKP changes: 38 1 1 1 OTKP changes: 38 1 1 1 OTKP changes: 38 1 1 1 Run 6 Omega scan: (-99.000 - -74.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 457 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: 0.066054 0.015575 0.006260 ( 0.000030 0.000072 0.000037 ) -0.016440 0.064770 0.012865 ( 0.000043 0.000101 0.000052 ) -0.003020 -0.014004 0.066599 ( 0.000027 0.000064 0.000033 ) M - matrix: 0.004642 0.000006 0.000001 ( 0.000004 0.000006 0.000003 ) 0.000006 0.004634 -0.000002 ( 0.000006 0.000013 0.000006 ) 0.000001 -0.000002 0.004640 ( 0.000003 0.000006 0.000005 ) Constraint UB - matrix: 0.066054 0.015575 0.006260 ( 0.000030 0.000072 0.000037 ) -0.016440 0.064770 0.012865 ( 0.000043 0.000101 0.000052 ) -0.003020 -0.014004 0.066599 ( 0.000027 0.000064 0.000033 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 38 obs out of 38 (total:38,skipped:0) (100.00%) unit cell: 10.410(6) 10.420(14) 10.413(6) 89.98(7) 90.01(4) 90.08(7) V = 1129(2) unit cell: 10.4142(16) 10.4142(16) 10.4142(16) 90.0 90.0 90.0 V = 1129.5(3) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068116 0.000014 -0.000068 ( 0.000009 0.000010 0.000010 ) -0.000013 0.068020 0.000017 ( 0.000010 0.000011 0.000010 ) 0.000033 -0.000022 0.068115 ( 0.000007 0.000008 0.000008 ) M - matrix: 0.004640 0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000000 0.004627 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000000 0.004640 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068116 0.000014 -0.000068 ( 0.000009 0.000010 0.000010 ) -0.000013 0.068020 0.000017 ( 0.000010 0.000011 0.000010 ) 0.000033 -0.000022 0.068115 ( 0.000007 0.000008 0.000008 ) M - matrix: 0.004636 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004636 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004636 ( 0.000000 0.000000 0.000000 ) UB fit with 1224 obs out of 1244 (total:1244,skipped:0) (98.39%) unit cell: 10.4131(14) 10.4278(16) 10.4133(12) 89.995(11) 89.971(10) 90.001(12) V = 1130.7(3) unit cell: 10.4181(4) 10.4181(4) 10.4181(4) 90.0 90.0 90.0 V = 1130.74(7) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 116 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof 5416 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:24:40 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.144) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.144) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.144) Run 6 Omega scan: (-99.000 - -74.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) PROFFIT INFO: signal sum: min=-775.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-614.5758 max=1271248.5683 PROFFIT INFO: background sum: min=-143.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=392.0000 max=6344.0000 PROFFIT INFO: num of signal pixels: min=42 max=557 PROFFIT INFO: Inet: min=-983.3213 max=2033997.8750 PROFFIT INFO: sig(Inet): min=52.0614 max=30685.9824 PROFFIT INFO: Inet/sig(Inet): min=-1.46 max=258.41 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 453 1828 2772 3342 3609 4193 4560 4782 5127 5356 5416 Percent 8.4 33.8 51.2 61.7 66.6 77.4 84.2 88.3 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5416 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 5416 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2033998- 131948 541 424007.30 77.94 100.00 131874- 4177 541 30188.52 19.95 100.00 4152- 2130 541 2951.87 7.23 97.60 2125- 1264 541 1638.60 3.91 52.87 1263- 844 541 1036.85 2.41 17.56 842- 563 541 695.46 1.78 8.69 563- 351 541 450.34 1.26 5.73 350- 159 541 254.04 0.75 0.92 158- 22 541 84.85 0.30 0.00 22- -983 547 -123.75 -0.24 0.00 ------------------------------------------------------------------------------------ 2033998- -983 5416 46067.18 11.52 38.29 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 541 114290.07 15.57 68.58 1.73- 1.26 541 89719.52 21.45 60.81 1.26- 1.09 541 61624.92 18.69 66.91 1.09- 0.97 541 56547.73 15.23 35.49 0.97- 0.88 541 16576.81 6.75 43.07 0.88- 0.81 541 52765.75 14.78 37.52 0.81- 0.76 541 18960.57 5.81 18.30 0.76- 0.71 541 21579.35 6.98 17.38 0.71- 0.67 541 25415.69 8.20 28.84 0.67- 0.63 547 3661.68 1.81 6.40 ------------------------------------------------------------------------------------ 6.00- 0.63 5416 46067.18 11.52 38.29 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:24:41 2019 Sorting 5416 observations 53 unique observations with > 7.00 F2/sig(F2) 5416 observations in 6 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 24 540 Total number of frames 540 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 11 frame = 1 scale 5416 observations in 6 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 9 50 6 0 2 53 Total number of frames 53 1318 observations > 7.00 F2/sig(F2) 1318 observations in 6 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 9 50 6 0 2 53 Total number of frames 53 Removing 'redundancy=1' reflections Average redundancy: 19.6 (Out of 1318 removed 7 = 1311, unique = 67) 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 1311 observations in 6 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 9 50 6 0 2 53 Total number of frames 53 67 unique data precomputed (should be 67) 67 unique data with 1311 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 19.6 (Out of 1311 removed 0 = 1311, unique = 67) 67 unique data precomputed (should be 67) 67 unique data with 1311 observations RMS deviation of equivalent data = 0.31246 Rint = 0.24864 5 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24175, wR= 0.33842 Trying model 1 (ne=2, no=0)... Results: Rint= 0.12190, wR= 0.18392, Acormin=0.496, Acormax=1.432, Acor_av=0.986 F test: Probability=1.000, F= 3.917 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11106, wR= 0.17024, Acormin=0.459, Acormax=1.487, Acor_av=0.946 F test: Probability=0.999, F= 1.202 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11149, wR= 0.17414, Acormin=0.526, Acormax=1.518, Acor_av=0.984 F test: Probability=0.000, F= 0.988 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10117, wR= 0.15584, Acormin=0.422, Acormax=1.616, Acor_av=0.945 F test: Probability=0.999, F= 1.196 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09000, wR= 0.14457, Acormin=0.506, Acormax=1.796, Acor_av=0.970 F test: Probability=1.000, F= 1.256 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10903, wR= 0.16803, Acormin=0.429, Acormax=1.537, Acor_av=0.959 F test: Probability=0.000, F= 0.680 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09764, wR= 0.15294, Acormin=0.409, Acormax=1.678, Acor_av=0.935 F test: Probability=0.000, F= 0.846 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08680, wR= 0.14164, Acormin=0.475, Acormax=1.819, Acor_av=0.965 F test: Probability=0.858, F= 1.064 Trying model 9 (ne=6, no=5)... Results: Rint= 0.14033, wR= 0.18667, Acormin=-0.097, Acormax=0.943, Acor_av=0.445 F test: Probability=0.000, F= 0.403 Final absorption model (ne=4, no=3): Rint= 0.09000, Acormin=0.506, Acormax=1.796, Acor_av=0.970 Combined refinement in use Rint: 0.25038 There are 53 active scales (one needs to be fixed) Refinement control: frame scale #46 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 76 pars with 2926 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31246 Using Levenberg-Marquardt: 0.00010 New wR= 0.10146 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24864 with corrections 0.07516 Rint for all data: 0.25038 with corrections 0.07786 4 observations identified as outliers and rejected Cycle 2 wR= 0.08813 Using Levenberg-Marquardt: 0.00001 New wR= 0.07452 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24758 with corrections 0.05515 Rint for all data: 0.25038 with corrections 0.06184 2 observations identified as outliers and rejected Cycle 3 wR= 0.06984 Using Levenberg-Marquardt: 0.00000 New wR= 0.06776 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24759 with corrections 0.05088 Rint for all data: 0.25038 with corrections 0.05859 0 observations identified as outliers and rejected Cycle 4 wR= 0.06776 Using Levenberg-Marquardt: 0.00000 New wR= 0.06668 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24759 with corrections 0.05000 Rint for all data: 0.25038 with corrections 0.05765 1 observations identified as outliers and rejected Cycle 5 wR= 0.06398 Using Levenberg-Marquardt: 0.00000 New wR= 0.06461 Using Levenberg-Marquardt: 0.00000 New wR= 0.06461 Using Levenberg-Marquardt: 0.00000 New wR= 0.06461 Using Levenberg-Marquardt: 0.00001 New wR= 0.06461 Using Levenberg-Marquardt: 0.00010 New wR= 0.06461 Using Levenberg-Marquardt: 0.00100 New wR= 0.06461 Using Levenberg-Marquardt: 0.01000 New wR= 0.06459 Using Levenberg-Marquardt: 0.10000 New wR= 0.06444 Using Levenberg-Marquardt: 1.00000 New wR= 0.06405 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24593 with corrections 0.04831 Rint for all data: 0.25038 with corrections 0.05662 Final wR= 0.06405 Final frame scales: Min= 0.7295 Max= 1.3406 Final absorption correction factors: Amin= 0.3595 Amax= 1.6713 PROFFIT INFO: Inet (after scale3 abspack): min=-1079.3871 max=1303698.8750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=40.3137 max=24532.7813 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/104 5416 reflections read from tmp file 211 reflections are rejected (210 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 4 5 6 5 5 5 6 201 Initial Chi^2= 0.53020 Cycle 1, Chi^2= 1.02882 Current error model SIG(F2)^2 = 70.71*I_RAW + 8.21*I_BACK+(0.03289*)^2 Cycle 2, Chi^2= 1.02079 Current error model SIG(F2)^2 = 86.32*I_RAW + 4.97*I_BACK+(0.02661*)^2 Cycle 3, Chi^2= 1.01027 Current error model SIG(F2)^2 = 92.92*I_RAW + 3.85*I_BACK+(0.02491*)^2 Cycle 4, Chi^2= 1.00395 Current error model SIG(F2)^2 = 95.43*I_RAW + 3.48*I_BACK+(0.02450*)^2 Cycle 5, Chi^2= 1.00135 Current error model SIG(F2)^2 = 96.31*I_RAW + 3.37*I_BACK+(0.02438*)^2 Cycle 6, Chi^2= 1.00044 Current error model SIG(F2)^2 = 96.61*I_RAW + 3.33*I_BACK+(0.02434*)^2 Cycle 7, Chi^2= 1.00014 Current error model SIG(F2)^2 = 96.70*I_RAW + 3.31*I_BACK+(0.02433*)^2 Final Chi^2= 1.00014 Final error model SIG(F2)^2 = 96.70*I_RAW + 3.31*I_BACK+(0.02433*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1303699- 117253 541 389717.24 31.80 100.00 116944- 3509 541 29826.26 12.76 100.00 3509- 2059 541 2733.40 5.94 98.15 2056- 1181 541 1547.13 3.84 61.74 1177- 793 541 970.91 2.71 23.11 792- 530 541 658.45 2.36 14.60 529- 335 541 430.10 1.98 8.69 335- 152 541 245.82 1.50 3.51 151- 22 541 84.27 0.80 0.37 22- -1079 547 -124.59 -0.52 0.00 ------------------------------------------------------------------------------------ 1303699- -1079 5416 42561.56 6.31 40.97 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 541 106407.80 10.27 71.72 1.73- 1.26 541 83302.28 9.75 63.40 1.26- 1.09 541 57290.36 8.30 70.43 1.09- 0.97 541 51728.59 6.84 36.23 0.97- 0.88 541 14417.93 4.54 47.69 0.88- 0.81 541 49643.16 7.77 42.33 0.81- 0.76 541 17516.12 3.81 20.33 0.76- 0.71 541 19324.33 4.81 19.22 0.71- 0.67 541 22984.11 5.36 31.24 0.67- 0.63 547 3434.85 1.70 7.50 ------------------------------------------------------------------------------------ 6.00- 0.63 5416 42561.56 6.31 40.97 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 541 106407.80 10.27 71.72 6.00- 1.26 1082 94855.04 10.01 67.56 6.00- 1.09 1623 82333.48 9.44 68.52 6.00- 0.97 2164 74682.26 8.79 60.44 6.00- 0.88 2705 62629.39 7.94 57.89 6.00- 0.81 3246 60465.02 7.91 55.30 6.00- 0.76 3787 54329.46 7.33 50.30 6.00- 0.71 4328 49953.82 7.01 46.42 6.00- 0.67 4869 46957.19 6.83 44.73 6.00- 0.63 5416 42561.56 6.31 40.97 ------------------------------------------------------------------------------------ 6.00- 0.63 5416 42561.56 6.31 40.97 Scale applied to data: s=0.767048 (maximum obs:1303698.875,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.057; Rsigma 0.037: data 5416 -> merged 240 With outlier rejection... Rint 0.049; Rsigma 0.037: data 5394 -> merged 240 Rejected total: 22, method kkm 16, method Blessing 6 Completeness direct cell (a, b, c) = (10.418, 10.418, 10.418), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627095, 6.014884 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.42 - 1.59 21 21 29.76 100.00 625 1.57 - 1.20 21 21 30.81 100.00 647 1.20 - 1.02 21 21 28.71 100.00 603 1.02 - 0.91 21 21 27.62 100.00 580 0.91 - 0.85 21 21 24.48 100.00 514 0.84 - 0.79 21 21 24.00 100.00 504 0.78 - 0.74 21 21 22.86 100.00 480 0.74 - 0.71 21 21 18.81 100.00 395 0.71 - 0.68 21 21 21.33 100.00 448 0.68 - 0.65 23 23 17.91 100.00 412 --------------------------------------------------------------- 10.42 - 0.65 212 212 24.57 100.00 5208 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:24:41 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.413129 10.427836 10.413296 89.9953 89.9713 90.0008 5394 Reflections read from file xs2212a.hkl 5361 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.29 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2693 0 3554 3551 5361 N (int>3sigma) = 0 0 0 0 1171 0 1551 1529 2202 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 32.9 30.8 32.1 Mean int/sigma = 0.0 0.0 0.0 0.0 3.9 0.0 6.4 6.3 6.3 Lattice type: F chosen Volume: 1130.74 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.361 7.365 7.368 60.02 60.03 90.00 Niggli form: a.a = 54.190 b.b = 54.245 c.c = 54.290 b.c = 27.121 a.c = 27.093 a.b = 0.001 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.160 CUBIC F-lattice R(int) = 0.049 [ 5130] Vol = 1130.7 Cell: 10.413 10.413 10.428 90.00 90.00 90.03 Volume: 1130.74 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.116 TETRAGONAL I-lattice R(int) = 0.048 [ 4745] Vol = 565.4 Cell: 7.368 7.368 10.413 90.02 89.98 89.92 Volume: 565.37 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.060 TETRAGONAL I-lattice R(int) = 0.048 [ 4745] Vol = 565.4 Cell: 7.361 7.365 10.428 90.00 90.00 90.00 Volume: 565.37 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.062 ORTHORHOMBIC F-lattice R(int) = 0.048 [ 4692] Vol = 1130.7 Cell: 10.413 10.413 10.428 90.00 90.00 89.97 Volume: 1130.74 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.129 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4671] Vol = 565.4 Cell: 10.413 7.368 7.368 89.92 89.98 90.02 Volume: 565.37 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.003 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 4674] Vol = 565.4 Cell: 7.361 7.365 10.428 90.00 90.00 90.00 Volume: 565.37 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.058 MONOCLINIC I-lattice R(int) = 0.046 [ 4148] Vol = 565.4 Cell: 7.368 10.413 7.369 90.02 90.08 90.02 Volume: 565.37 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.057 MONOCLINIC I-lattice R(int) = 0.045 [ 4151] Vol = 565.4 Cell: 7.368 10.413 7.368 90.02 90.08 90.02 Volume: 565.37 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.002 MONOCLINIC I-lattice R(int) = 0.044 [ 4126] Vol = 565.4 Cell: 7.365 7.361 10.428 90.00 90.00 90.00 Volume: 565.37 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.002 MONOCLINIC I-lattice R(int) = 0.044 [ 4141] Vol = 565.4 Cell: 7.361 7.365 10.428 90.00 90.00 90.00 Volume: 565.37 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 3098] Vol = 282.7 Cell: 7.361 7.365 7.368 60.02 60.03 90.00 Volume: 282.69 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -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 2693 0 3565 3551 5361 N (int>3sigma) = 0 0 0 0 1171 0 1561 1529 2202 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 31.5 30.8 32.1 Mean int/sigma = 0.0 0.0 0.0 0.0 3.9 0.0 6.3 6.3 6.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.168 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 38 38 400 1051 N I>3s 2 2 2 559 0.0 0.0 0.0 2.0 0.9 0.9 0.3 4.9 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 0.049 4758 Fd-3m 1 1 227 C N N N N 37 2284 0.049 4820 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.413296 10.413129 10.427836 90.0008 90.0047 90.0287 ZERR 5.00 0.001183 0.001427 0.001610 0.0118 0.0109 0.0103 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1170816- 130148 537 525 26 20.2 389304.02 31.79 0.044 0.057 110955- 3247 610 608 26 23.4 27726.85 12.04 0.065 0.077 3052- 1398 793 790 26 30.4 2260.49 5.37 0.129 0.187 1365- 888 682 682 26 26.2 1072.21 2.70 0.231 0.300 844- 507 661 661 26 25.4 661.20 2.41 0.294 0.408 503- 317 627 627 26 24.1 393.80 1.67 0.436 0.595 306- 157 512 512 26 19.7 238.65 1.36 0.552 0.819 154- 39 552 551 26 21.2 79.23 0.59 0.872 2.242 34- -135 442 438 32 13.7 -18.53 -0.02 0.998 4.752 ------------------------------------------------------------------------------------------- 1170816- -135 5416 5394 240 22.5 41639.09 6.26 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-1.44 805 800 26 30.8 116131.48 11.36 0.043 0.054 0.027 1.39-1.09 827 824 26 31.7 43485.85 7.25 0.046 0.056 0.034 1.06-0.94 692 690 26 26.5 40329.75 5.84 0.047 0.056 0.035 0.92-0.85 654 653 26 25.1 42540.25 7.45 0.052 0.071 0.041 0.84-0.78 638 635 26 24.4 24645.66 4.98 0.054 0.068 0.047 0.78-0.73 565 565 27 20.9 13262.27 3.76 0.072 0.090 0.064 0.72-0.69 548 546 26 21.0 14713.68 3.88 0.069 0.076 0.068 0.68-0.66 491 489 27 18.1 15209.75 3.90 0.075 0.102 0.068 0.65-0.63 196 192 30 6.4 8557.37 2.49 0.084 0.086 0.086 ------------------------------------------------------------------------------------------------------ inf-0.63 5416 5394 240 22.5 41639.09 6.26 0.049 0.062 0.037 inf-0.65 5224 5206 211 24.7 42899.52 6.41 0.049 0.061 0.036 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-1.44 800 26 26 100.0 30.8 116131.48 63.28 0.043 0.006 1.39-1.09 824 26 26 100.0 31.7 43485.85 36.87 0.046 0.007 1.06-0.94 690 26 26 100.0 26.5 40329.75 31.26 0.047 0.008 0.92-0.85 653 26 26 100.0 25.1 42540.25 36.80 0.052 0.009 0.84-0.78 635 26 26 100.0 24.4 24645.66 23.33 0.054 0.010 0.78-0.73 565 27 27 100.0 20.9 13262.27 17.17 0.072 0.015 0.72-0.69 546 26 26 100.0 21.0 14713.68 16.66 0.069 0.016 0.68-0.66 489 27 27 100.0 18.1 15209.75 18.26 0.075 0.016 0.65-0.63 192 30 30 100.0 6.4 8557.37 6.25 0.084 0.037 -------------------------------------------------------------------------------------------- inf-0.63 5394 240 240 100.0 22.5 41639.09 31.58 0.049 0.009 inf-0.65 5206 211 211 100.0 24.7 42899.52 32.52 0.049 0.008 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066087 0.014948 0.006894 ( 0.000009 0.000010 0.000010 ) -0.016078 0.064774 0.013188 ( 0.000010 0.000010 0.000010 ) -0.003696 -0.014405 0.066469 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004640 -0.000000 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000000 0.004627 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000000 0.004640 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066087 0.014948 0.006894 ( 0.000009 0.000010 0.000010 ) -0.016078 0.064774 0.013188 ( 0.000010 0.000010 0.000010 ) -0.003696 -0.014405 0.066469 ( 0.000008 0.000008 0.000008 ) M - matrix: 0.004636 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004636 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004636 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4132(14) 10.4280(16) 10.4133(12) 89.998(11) 89.974(10) 89.997(12) V = 1130.8(3) unit cell: 10.4182(4) 10.4182(4) 10.4182(4) 90.0 90.0 90.0 V = 1130.77(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.144) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.144) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.144) Run 6 Omega scan: (-99.000 - -74.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) PROFFIT INFO: signal sum: min=-775.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-614.5758 max=1271248.5683 PROFFIT INFO: background sum: min=-143.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=392.0000 max=6344.0000 PROFFIT INFO: num of signal pixels: min=42 max=557 PROFFIT INFO: Inet: min=-983.3213 max=2033997.8750 PROFFIT INFO: sig(Inet): min=52.0614 max=30685.9824 PROFFIT INFO: Inet/sig(Inet): min=-1.46 max=258.41 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 906 3656 5544 6684 7218 8386 9120 9564 10254 10712 10832 Percent 8.4 33.8 51.2 61.7 66.6 77.4 84.2 88.3 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5416 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 5416 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2033998- 131948 541 424007.30 77.94 100.00 131874- 4177 541 30188.52 19.95 100.00 4152- 2130 541 2951.87 7.23 97.60 2125- 1264 541 1638.60 3.91 52.87 1263- 844 541 1036.85 2.41 17.56 842- 563 541 695.46 1.78 8.69 563- 351 541 450.34 1.26 5.73 350- 159 541 254.04 0.75 0.92 158- 22 541 84.85 0.30 0.00 22- -983 547 -123.75 -0.24 0.00 ------------------------------------------------------------------------------------ 2033998- -983 5416 46067.18 11.52 38.29 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 541 114290.07 15.57 68.58 1.73- 1.26 541 89719.52 21.45 60.81 1.26- 1.09 541 61624.92 18.69 66.91 1.09- 0.97 541 56547.73 15.23 35.49 0.97- 0.88 541 16576.81 6.75 43.07 0.88- 0.81 541 52765.75 14.78 37.52 0.81- 0.76 541 18960.57 5.81 18.30 0.76- 0.71 541 21579.35 6.98 17.38 0.71- 0.67 541 25415.69 8.20 28.84 0.67- 0.63 547 3661.68 1.81 6.40 ------------------------------------------------------------------------------------ 6.00- 0.63 5416 46067.18 11.52 38.29 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:24:42 2019 Sorting 5416 observations 43 unique observations with > 7.00 F2/sig(F2) 5416 observations in 6 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 24 540 Total number of frames 540 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 13 frame = 1 scale 5416 observations in 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 1 42 Total number of frames 42 1318 observations > 7.00 F2/sig(F2) 1318 observations in 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 1 42 Total number of frames 42 Removing 'redundancy=1' reflections Average redundancy: 23.9 (Out of 1318 removed 3 = 1315, unique = 55) 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 1315 observations in 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 1 42 Total number of frames 42 55 unique data precomputed (should be 55) 55 unique data with 1315 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.9 (Out of 1315 removed 0 = 1315, unique = 55) 55 unique data precomputed (should be 55) 55 unique data with 1315 observations RMS deviation of equivalent data = 0.31279 Rint = 0.24871 5 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24182, wR= 0.33869 Trying model 1 (ne=2, no=0)... Results: Rint= 0.12185, wR= 0.18446, Acormin=0.497, Acormax=1.431, Acor_av=0.986 F test: Probability=1.000, F= 3.923 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11112, wR= 0.17092, Acormin=0.458, Acormax=1.485, Acor_av=0.945 F test: Probability=0.999, F= 1.200 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11101, wR= 0.17488, Acormin=0.526, Acormax=1.517, Acor_av=0.985 F test: Probability=0.000, F= 0.997 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10135, wR= 0.15649, Acormin=0.423, Acormax=1.618, Acor_av=0.946 F test: Probability=0.999, F= 1.193 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09010, wR= 0.14529, Acormin=0.507, Acormax=1.801, Acor_av=0.971 F test: Probability=1.000, F= 1.258 Final absorption model (ne=4, no=3): Rint= 0.09010, Acormin=0.507, Acormax=1.801, Acor_av=0.971 Combined refinement in use Rint: 0.25047 There are 42 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 65 pars with 2145 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31279 Using Levenberg-Marquardt: 0.00010 New wR= 0.10880 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24871 with corrections 0.07740 Rint for all data: 0.25047 with corrections 0.08014 2 observations identified as outliers and rejected Cycle 2 wR= 0.10124 Using Levenberg-Marquardt: 0.00001 New wR= 0.08940 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24784 with corrections 0.06204 Rint for all data: 0.25047 with corrections 0.06757 2 observations identified as outliers and rejected Cycle 3 wR= 0.08347 Using Levenberg-Marquardt: 0.00000 New wR= 0.08243 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24691 with corrections 0.05725 Rint for all data: 0.25047 with corrections 0.06317 0 observations identified as outliers and rejected Cycle 4 wR= 0.08243 Using Levenberg-Marquardt: 0.00000 New wR= 0.08111 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24691 with corrections 0.05697 Rint for all data: 0.25047 with corrections 0.06288 0 observations identified as outliers and rejected Cycle 5 wR= 0.08111 Using Levenberg-Marquardt: 0.00000 New wR= 0.08050 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.24691 with corrections 0.05641 Rint for all data: 0.25047 with corrections 0.06227 0 observations identified as outliers and rejected Final wR= 0.08050 Final frame scales: Min= 0.6761 Max= 1.1649 Final absorption correction factors: Amin= 0.3770 Amax= 1.6124 PROFFIT INFO: Inet (after scale3 abspack): min=-1101.4661 max=1310620.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.0151 max=24479.4551 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/104 5416 reflections read from tmp file 245 reflections are rejected (245 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 2 5 3 2 1 4 5 140 Initial Chi^2= 0.52852 Cycle 1, Chi^2= 1.00725 Current error model SIG(F2)^2 = 67.26*I_RAW + 9.84*I_BACK+(0.03631*)^2 Cycle 2, Chi^2= 1.01771 Current error model SIG(F2)^2 = 84.58*I_RAW + 5.67*I_BACK+(0.02803*)^2 Cycle 3, Chi^2= 1.01068 Current error model SIG(F2)^2 = 92.51*I_RAW + 4.20*I_BACK+(0.02560*)^2 Cycle 4, Chi^2= 1.00395 Current error model SIG(F2)^2 = 95.39*I_RAW + 3.75*I_BACK+(0.02510*)^2 Cycle 5, Chi^2= 1.00117 Current error model SIG(F2)^2 = 96.28*I_RAW + 3.63*I_BACK+(0.02499*)^2 Cycle 6, Chi^2= 1.00032 Current error model SIG(F2)^2 = 96.53*I_RAW + 3.59*I_BACK+(0.02497*)^2 Cycle 7, Chi^2= 1.00009 Current error model SIG(F2)^2 = 96.60*I_RAW + 3.58*I_BACK+(0.02496*)^2 Final Chi^2= 1.00009 Final error model SIG(F2)^2 = 96.60*I_RAW + 3.58*I_BACK+(0.02496*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1310621- 118512 541 390203.07 31.30 100.00 117995- 3560 541 29594.82 12.71 100.00 3558- 2091 541 2730.10 5.97 98.52 2086- 1173 541 1551.34 3.81 61.55 1173- 793 541 970.29 2.71 22.37 792- 530 541 657.23 2.37 14.60 527- 335 541 429.29 1.95 8.13 335- 151 541 245.10 1.51 3.88 151- 22 541 83.92 0.79 0.18 22- -1101 547 -124.55 -0.51 0.00 ------------------------------------------------------------------------------------ 1310621- -1101 5416 42586.69 6.25 40.88 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 541 106744.02 10.15 71.72 1.73- 1.26 541 83405.00 9.65 63.22 1.26- 1.09 541 57427.16 8.21 70.06 1.09- 0.97 541 51641.00 6.77 36.23 0.97- 0.88 541 14484.05 4.51 47.69 0.88- 0.81 541 49624.93 7.70 42.14 0.81- 0.76 541 17501.32 3.78 20.33 0.76- 0.71 541 19259.06 4.78 19.22 0.71- 0.67 541 22816.58 5.34 31.05 0.67- 0.63 547 3398.42 1.70 7.50 ------------------------------------------------------------------------------------ 6.00- 0.63 5416 42586.69 6.25 40.88 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 541 106744.02 10.15 71.72 6.00- 1.26 1082 95074.51 9.90 67.47 6.00- 1.09 1623 82525.39 9.34 68.33 6.00- 0.97 2164 74804.30 8.69 60.30 6.00- 0.88 2705 62740.25 7.86 57.78 6.00- 0.81 3246 60554.36 7.83 55.18 6.00- 0.76 3787 54403.93 7.25 50.20 6.00- 0.71 4328 50010.82 6.94 46.33 6.00- 0.67 4869 46989.24 6.77 44.63 6.00- 0.63 5416 42586.69 6.25 40.88 ------------------------------------------------------------------------------------ 6.00- 0.63 5416 42586.69 6.25 40.88 Scale applied to data: s=0.762996 (maximum obs:1310620.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.062; Rsigma 0.037: data 5416 -> merged 162 With outlier rejection... Rint 0.054; Rsigma 0.037: data 5396 -> merged 162 Rejected total: 20, method kkm 11, method Blessing 9 Completeness direct cell (a, b, c) = (10.418, 10.418, 10.418), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.627100, 6.014929 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.42 - 1.76 14 14 35.43 100.00 496 1.74 - 1.27 14 14 38.93 100.00 545 1.26 - 1.06 14 14 43.86 100.00 614 1.05 - 0.97 14 14 38.07 100.00 533 0.95 - 0.88 14 14 39.64 100.00 555 0.87 - 0.81 14 14 35.50 100.00 497 0.80 - 0.76 14 14 37.07 100.00 519 0.76 - 0.72 14 14 30.79 100.00 431 0.72 - 0.69 14 14 34.21 100.00 479 0.69 - 0.65 19 19 28.47 100.00 541 --------------------------------------------------------------- 10.42 - 0.65 145 145 35.93 100.00 5210 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:24:41 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.413129 10.427836 10.413296 89.9953 89.9713 90.0008 5394 Reflections read from file xs2212a.hkl 5361 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.29 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2693 0 3554 3551 5361 N (int>3sigma) = 0 0 0 0 1171 0 1551 1529 2202 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 32.9 30.8 32.1 Mean int/sigma = 0.0 0.0 0.0 0.0 3.9 0.0 6.4 6.3 6.3 Lattice type: F chosen Volume: 1130.74 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.361 7.365 7.368 60.02 60.03 90.00 Niggli form: a.a = 54.190 b.b = 54.245 c.c = 54.290 b.c = 27.121 a.c = 27.093 a.b = 0.001 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.160 CUBIC F-lattice R(int) = 0.049 [ 5130] Vol = 1130.7 Cell: 10.413 10.413 10.428 90.00 90.00 90.03 Volume: 1130.74 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.116 TETRAGONAL I-lattice R(int) = 0.048 [ 4745] Vol = 565.4 Cell: 7.368 7.368 10.413 90.02 89.98 89.92 Volume: 565.37 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.060 TETRAGONAL I-lattice R(int) = 0.048 [ 4745] Vol = 565.4 Cell: 7.361 7.365 10.428 90.00 90.00 90.00 Volume: 565.37 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.062 ORTHORHOMBIC F-lattice R(int) = 0.048 [ 4692] Vol = 1130.7 Cell: 10.413 10.413 10.428 90.00 90.00 89.97 Volume: 1130.74 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.129 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4671] Vol = 565.4 Cell: 10.413 7.368 7.368 89.92 89.98 90.02 Volume: 565.37 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.003 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 4674] Vol = 565.4 Cell: 7.361 7.365 10.428 90.00 90.00 90.00 Volume: 565.37 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.058 MONOCLINIC I-lattice R(int) = 0.046 [ 4148] Vol = 565.4 Cell: 7.368 10.413 7.369 90.02 90.08 90.02 Volume: 565.37 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.057 MONOCLINIC I-lattice R(int) = 0.045 [ 4151] Vol = 565.4 Cell: 7.368 10.413 7.368 90.02 90.08 90.02 Volume: 565.37 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.002 MONOCLINIC I-lattice R(int) = 0.044 [ 4126] Vol = 565.4 Cell: 7.365 7.361 10.428 90.00 90.00 90.00 Volume: 565.37 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.002 MONOCLINIC I-lattice R(int) = 0.044 [ 4141] Vol = 565.4 Cell: 7.361 7.365 10.428 90.00 90.00 90.00 Volume: 565.37 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 3098] Vol = 282.7 Cell: 7.361 7.365 7.368 60.02 60.03 90.00 Volume: 282.69 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -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 2693 0 3565 3551 5361 N (int>3sigma) = 0 0 0 0 1171 0 1561 1529 2202 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 31.5 30.8 32.1 Mean int/sigma = 0.0 0.0 0.0 0.0 3.9 0.0 6.3 6.3 6.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.168 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 38 38 400 1051 N I>3s 2 2 2 559 0.0 0.0 0.0 2.0 0.9 0.9 0.3 4.9 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 0.049 4758 Fd-3m 1 1 227 C N N N N 37 2284 0.049 4820 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.413296 10.413129 10.427836 90.0008 90.0047 90.0287 ZERR 5.00 0.001183 0.001427 0.001610 0.0118 0.0109 0.0103 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1178119- 92902 658 644 27 23.9 337647.34 29.26 0.050 0.063 78193- 1856 1023 1020 27 37.8 5379.20 8.02 0.088 0.095 1724- 787 1095 1094 27 40.5 1145.93 2.88 0.223 0.301 783- 325 1109 1109 27 41.1 497.91 2.04 0.356 0.491 322- 79 746 744 27 27.6 207.45 1.12 0.629 1.018 64- -116 785 785 27 29.1 14.63 0.23 0.961 4.448 ------------------------------------------------------------------------------------------- 1178119- -116 5416 5396 162 33.3 41679.64 6.20 0.054 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-1.27 1045 1039 27 38.5 95699.98 10.09 0.046 0.057 0.028 1.26-0.97 1095 1090 27 40.4 52479.01 7.29 0.050 0.065 0.034 0.97-0.81 1083 1081 28 38.6 31996.89 6.09 0.063 0.083 0.043 0.81-0.73 958 957 28 34.2 17522.00 4.16 0.063 0.080 0.056 0.72-0.67 826 824 27 30.5 18521.94 4.52 0.075 0.095 0.064 0.66-0.63 409 405 25 16.2 4073.23 1.82 0.109 0.084 0.125 ------------------------------------------------------------------------------------------------------ inf-0.63 5416 5396 162 33.3 41679.64 6.20 0.054 0.067 0.037 inf-0.65 5224 5208 144 36.2 42962.29 6.35 0.053 0.066 0.037 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-1.27 1039 27 27 100.0 38.5 95699.98 59.70 0.046 0.007 1.26-0.97 1090 27 27 100.0 40.4 52479.01 43.58 0.050 0.006 0.97-0.81 1081 28 28 100.0 38.6 31996.89 37.48 0.063 0.009 0.81-0.73 957 28 28 100.0 34.2 17522.00 22.05 0.063 0.011 0.72-0.67 824 27 27 100.0 30.5 18521.94 26.69 0.075 0.012 0.66-0.63 405 25 25 100.0 16.2 4073.23 7.52 0.109 0.035 -------------------------------------------------------------------------------------------- inf-0.63 5396 162 162 100.0 33.3 41679.64 36.36 0.054 0.008 inf-0.65 5208 144 144 100.0 36.2 42962.29 37.45 0.053 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:31:04 2019) ID: 3668; threads 40; handles 811; mem 514516.00 (1204692.00)kB; time: 1w 5d 0h 41m 52s MEMORY INFO: Memory PF:217.0, Ph:552.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.5,peak PF: 700.2, WS: 471.1, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:219.0, Ph:553.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.3,peak PF: 700.2, WS: 472.9, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:31:04 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000016 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000014 0.000013 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000016 0.000015 ) 10.42433 ( 0.00232 ) 10.43788 ( 0.00217 ) 10.40727 ( 0.00234 ) 89.88512 ( 0.01767 ) 89.79539 ( 0.01816 ) 90.20497 ( 0.01771 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:31:04 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000016 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000014 0.000013 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000016 0.000015 ) M - matrix: 0.004635 0.000003 -0.000010 ( 0.000002 0.000001 0.000001 ) 0.000003 0.004622 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000010 -0.000003 0.004650 ( 0.000001 0.000001 0.000002 ) unit cell: 10.424(2) 10.438(2) 10.407(2) 89.885(18) 89.795(18) 90.205(18) V = 1132.4(4) unit cell: 10.4177(8) 10.4177(8) 10.4177(8) 90.0 90.0 90.0 V = 1130.60(14) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 218 peaks identified as outliers and rejected 218 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 218 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 218 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.60 | 22 | 0.998 ( 0.544) | 0.879 ( 0.218) | 1.641 ( 2.386) | 2.60- 1.76 | 22 | 0.823 ( 0.086) | 0.809 ( 0.143) | 0.780 ( 0.409) | 1.76- 1.57 | 22 | 0.861 ( 0.093) | 0.897 ( 0.150) | 0.733 ( 0.321) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.973 ( 0.138) | 1.034 ( 0.496) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.033 ( 0.124) | 1.027 ( 0.679) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.939 ( 0.170) | 0.931 ( 0.396) | 1.00- 0.88 | 22 | 0.960 ( 0.074) | 1.004 ( 0.125) | 1.180 ( 0.494) | 0.88- 0.79 | 22 | 0.984 ( 0.058) | 1.025 ( 0.139) | 1.235 ( 0.386) | 0.79- 0.70 | 22 | 0.979 ( 0.045) | 0.955 ( 0.108) | 1.275 ( 0.476) | 0.69- 0.63 | 20 | 0.944 ( 0.037) | 0.926 ( 0.079) | 1.305 ( 0.483) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 218 | 0.933 ( 0.193) | 0.944 ( 0.159) | 1.112 ( 0.916) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.87 | 25 | 0.945 ( 0.067) | 0.936 ( 0.094) | 1.074 ( 0.403) | 0.86- 0.73 | 25 | 0.958 ( 0.050) | 0.919 ( 0.091) | 1.335 ( 0.450) | 0.73- 0.63 | 29 | 0.929 ( 0.037) | 0.880 ( 0.095) | 1.340 ( 0.463) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 254 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.061 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 238 peaks identified as outliers and rejected 238 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 238 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 238 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.999 ( 0.045) | 0.990 ( 0.123) | 1.316 ( 0.487) | 0.69- 0.63 | 22 | 0.974 ( 0.053) | 0.912 ( 0.110) | 1.255 ( 0.524) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 238 | 0.950 ( 0.083) | 0.961 ( 0.132) | 1.035 ( 0.512) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 277 peaks identified as outliers and rejected 277 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 277 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 277 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.956 ( 0.112) | 0.968 ( 0.143) | 0.954 ( 0.380) | 1.56- 1.35 | 28 | 0.959 ( 0.097) | 0.971 ( 0.157) | 0.802 ( 0.335) | 1.35- 1.19 | 28 | 0.939 ( 0.098) | 0.977 ( 0.159) | 0.717 ( 0.268) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.016 ( 0.108) | 0.880 ( 0.347) | 1.06- 0.91 | 28 | 1.003 ( 0.076) | 1.052 ( 0.122) | 0.969 ( 0.382) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 0.999 ( 0.122) | 1.085 ( 0.341) | 0.86- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.132) | 1.179 ( 0.466) | 0.73- 0.63 | 25 | 1.004 ( 0.041) | 1.024 ( 0.127) | 1.077 ( 0.358) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 277 | 0.968 ( 0.099) | 0.990 ( 0.176) | 0.949 ( 0.406) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 276 obs out of 277 (total:277,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064852 0.013482 ( 0.000023 0.000017 0.000018 ) -0.002784 -0.014648 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000002 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000002 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 276 1 1 1 OTKP changes: 276 1 1 1 OTKP changes: 276 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000017 0.000012 0.000013 ) -0.016328 0.064755 0.013398 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066457 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000017 0.000012 0.000013 ) -0.016328 0.064755 0.013398 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066457 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 276 obs out of 277 (total:277,skipped:0) (99.64%) unit cell: 10.431(2) 10.410(2) 10.4177(19) 89.887(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000017 0.000012 0.000013 ) -0.016328 0.064755 0.013398 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066457 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000017 0.000012 0.000013 ) -0.016328 0.064755 0.013398 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066457 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 276 obs out of 277 (total:277,skipped:0) (99.64%) unit cell: 10.431(2) 10.410(2) 10.4177(19) 89.887(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 276 obs out of 277 (total:277,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 272 peaks identified as outliers and rejected 272 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 272 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 272 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.57 | 27 | 0.974 ( 0.112) | 0.999 ( 0.142) | 1.004 ( 0.427) | 1.50- 1.35 | 27 | 0.963 ( 0.092) | 0.979 ( 0.160) | 0.818 ( 0.386) | 1.35- 1.19 | 27 | 0.940 ( 0.103) | 0.968 ( 0.154) | 0.731 ( 0.285) | 1.19- 1.06 | 27 | 0.978 ( 0.066) | 1.024 ( 0.101) | 0.888 ( 0.347) | 1.06- 0.92 | 27 | 1.010 ( 0.075) | 1.070 ( 0.119) | 0.971 ( 0.376) | 0.92- 0.87 | 27 | 1.005 ( 0.061) | 0.992 ( 0.113) | 1.132 ( 0.382) | 0.87- 0.73 | 27 | 1.043 ( 0.052) | 1.032 ( 0.132) | 1.207 ( 0.468) | 0.73- 0.63 | 29 | 1.001 ( 0.040) | 1.014 ( 0.123) | 1.092 ( 0.393) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 272 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.965 ( 0.413) | 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_6_26.rpb PROFFITPEAK info: 139 peaks in the peak location table UB fit with 45 obs out of 88 (total:88,skipped:0) (51.14%) UB - matrix: 0.066160 0.014953 0.006379 ( 0.000098 0.000207 0.000099 ) -0.016139 0.064573 0.013277 ( 0.000103 0.000217 0.000104 ) -0.003751 -0.014325 0.066507 ( 0.000104 0.000220 0.000105 ) M - matrix: 0.004652 0.000001 -0.000042 ( 0.000013 0.000016 0.000010 ) 0.000001 0.004598 0.000000 ( 0.000016 0.000029 0.000017 ) -0.000042 0.000000 0.004640 ( 0.000010 0.000017 0.000014 ) unit cell: 10.400(17) 10.46(3) 10.413(18) 90.0(2) 89.49(14) 90.01(19) V = 1133(4) UB fit with 45 obs out of 88 (total:88,skipped:0) (51.14%) UB - matrix: 0.066160 0.014953 0.006379 ( 0.000098 0.000207 0.000099 ) -0.016139 0.064573 0.013277 ( 0.000103 0.000217 0.000104 ) -0.003751 -0.014325 0.066507 ( 0.000104 0.000220 0.000105 ) M - matrix: 0.004652 0.000001 -0.000042 ( 0.000013 0.000016 0.000010 ) 0.000001 0.004598 0.000000 ( 0.000016 0.000029 0.000017 ) -0.000042 0.000000 0.004640 ( 0.000010 0.000017 0.000014 ) unit cell: 10.400(17) 10.46(3) 10.413(18) 90.0(2) 89.49(14) 90.01(19) V = 1133(4) OTKP changes: 35 1 1 1 OTKP changes: 35 1 1 1 OTKP changes: 35 1 1 1 No constraint UB - matrix: 0.065892 0.015476 0.006182 ( 0.000056 0.000087 0.000049 ) -0.016481 0.064427 0.012870 ( 0.000066 0.000103 0.000057 ) -0.002973 -0.014088 0.066493 ( 0.000038 0.000059 0.000033 ) M - matrix: 0.004622 -0.000000 -0.000002 ( 0.000008 0.000007 0.000004 ) -0.000000 0.004589 -0.000012 ( 0.000007 0.000014 0.000006 ) -0.000002 -0.000012 0.004625 ( 0.000004 0.000006 0.000005 ) Constraint UB - matrix: 0.065892 0.015476 0.006182 ( 0.000056 0.000087 0.000049 ) -0.016481 0.064427 0.012870 ( 0.000066 0.000103 0.000057 ) -0.002973 -0.014088 0.066493 ( 0.000038 0.000059 0.000033 ) M - matrix: 0.004617 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004617 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004617 ( 0.000000 0.000000 0.000002 ) UB fit with 82 obs out of 88 (total:88,skipped:0) (93.18%) unit cell: 10.433(9) 10.471(15) 10.430(6) 89.85(7) 89.97(6) 90.00(9) V = 1139(2) unit cell: 10.444(3) 10.444(3) 10.444(3) 90.0 90.0 90.0 V = 1139.3(5) UB fit with 82 obs out of 88 (total:88,skipped:0) (93.18%) UB - matrix: 0.065892 0.015476 0.006182 ( 0.000056 0.000087 0.000049 ) -0.016481 0.064427 0.012870 ( 0.000066 0.000103 0.000057 ) -0.002973 -0.014089 0.066493 ( 0.000038 0.000059 0.000033 ) M - matrix: 0.004622 -0.000000 -0.000002 ( 0.000008 0.000007 0.000004 ) -0.000000 0.004589 -0.000012 ( 0.000007 0.000014 0.000006 ) -0.000002 -0.000012 0.004625 ( 0.000004 0.000006 0.000005 ) unit cell: 10.433(9) 10.471(15) 10.430(6) 89.85(7) 89.97(6) 90.00(9) V = 1139(2) OTKP changes: 41 1 1 1 OTKP changes: 41 1 1 1 No constraint UB - matrix: 0.066054 0.015442 0.006203 ( 0.000054 0.000084 0.000047 ) -0.016469 0.064587 0.012865 ( 0.000066 0.000104 0.000058 ) -0.003005 -0.014146 0.066606 ( 0.000039 0.000061 0.000034 ) M - matrix: 0.004643 -0.000001 -0.000002 ( 0.000007 0.000007 0.000004 ) -0.000001 0.004610 -0.000015 ( 0.000007 0.000014 0.000006 ) -0.000002 -0.000015 0.004640 ( 0.000004 0.000006 0.000005 ) Constraint UB - matrix: 0.066054 0.015442 0.006203 ( 0.000054 0.000084 0.000047 ) -0.016469 0.064587 0.012865 ( 0.000066 0.000104 0.000058 ) -0.003005 -0.014146 0.066606 ( 0.000039 0.000061 0.000034 ) M - matrix: 0.004635 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004635 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004635 ( 0.000000 0.000000 0.000002 ) UB fit with 82 obs out of 88 (total:88,skipped:0) (93.18%) unit cell: 10.409(9) 10.447(15) 10.413(6) 89.81(7) 89.97(6) 89.99(9) V = 1132(2) unit cell: 10.423(3) 10.423(3) 10.423(3) 90.0 90.0 90.0 V = 1132.3(5) 88 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Run 6 Omega scan: (-99.000 - -49.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 753 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 82 obs out of 88 (total:88,skipped:0) (93.18%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_26.rpb 0 of 85 peaks identified as outliers and rejected 85 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 85 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 85 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 3.11 | 9 | 0.856 ( 0.133) | 0.863 ( 0.181) | 0.743 ( 0.244) | 3.00- 1.76 | 9 | 0.853 ( 0.110) | 0.887 ( 0.169) | 0.771 ( 0.369) | 1.76- 1.58 | 9 | 0.812 ( 0.087) | 0.807 ( 0.121) | 0.744 ( 0.275) | 1.57- 1.36 | 9 | 0.984 ( 0.053) | 1.034 ( 0.077) | 0.977 ( 0.129) | 1.36- 1.06 | 9 | 0.979 ( 0.108) | 1.007 ( 0.165) | 0.851 ( 0.410) | 1.06- 0.92 | 9 | 0.982 ( 0.069) | 1.002 ( 0.151) | 1.073 ( 0.313) | 0.88- 0.79 | 9 | 1.029 ( 0.043) | 1.048 ( 0.127) | 1.037 ( 0.382) | 0.79- 0.72 | 9 | 0.997 ( 0.037) | 0.922 ( 0.070) | 1.158 ( 0.504) | 0.72- 0.68 | 9 | 0.984 ( 0.034) | 0.892 ( 0.072) | 1.076 ( 0.493) | 0.68- 0.63 | 4 | 0.909 ( 0.028) | 0.840 ( 0.032) | 1.192 ( 0.322) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 85 | 0.940 ( 0.108) | 0.935 ( 0.153) | 0.948 ( 0.396) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 85 obs out of 85 (total:85,skipped:0) (100.00%) UB - matrix: 0.065968 0.015527 0.006274 ( 0.000033 0.000048 0.000032 ) -0.016438 0.064707 0.012963 ( 0.000037 0.000054 0.000035 ) -0.002870 -0.014094 0.066565 ( 0.000031 0.000046 0.000030 ) M - matrix: 0.004630 0.000001 0.000010 ( 0.000005 0.000004 0.000003 ) 0.000001 0.004627 -0.000002 ( 0.000004 0.000007 0.000004 ) 0.000010 -0.000002 0.004638 ( 0.000003 0.000004 0.000004 ) unit cell: 10.424(5) 10.428(8) 10.415(5) 89.98(5) 90.12(4) 90.01(5) V = 1132(1) OTKP changes: 85 1 1 1 OTKP changes: 85 1 1 1 No constraint UB - matrix: 0.066184 0.015499 0.006306 ( 0.000024 0.000036 0.000023 ) -0.016441 0.064842 0.012909 ( 0.000034 0.000049 0.000032 ) -0.003002 -0.014221 0.066735 ( 0.000022 0.000032 0.000021 ) M - matrix: 0.004660 0.000002 0.000005 ( 0.000003 0.000003 0.000002 ) 0.000002 0.004647 -0.000014 ( 0.000003 0.000007 0.000003 ) 0.000005 -0.000014 0.004660 ( 0.000002 0.000003 0.000003 ) Constraint UB - matrix: 0.066184 0.015499 0.006306 ( 0.000024 0.000036 0.000023 ) -0.016441 0.064842 0.012909 ( 0.000034 0.000049 0.000032 ) -0.003002 -0.014221 0.066735 ( 0.000022 0.000032 0.000021 ) M - matrix: 0.004658 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004658 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004658 ( 0.000000 0.000000 0.000001 ) UB fit with 85 obs out of 85 (total:85,skipped:0) (100.00%) unit cell: 10.391(4) 10.405(7) 10.391(3) 89.82(4) 90.06(3) 90.03(4) V = 1123.4(10) unit cell: 10.3955(9) 10.3955(9) 10.3955(9) 90.0 90.0 90.0 V = 1123.41(18) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - -49.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=52.904) HKL list info: 755 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 85 obs out of 85 (total:85,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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_26.rpb 0 of 86 peaks identified as outliers and rejected 86 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 86 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 86 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 2.99 | 9 | 0.861 ( 0.135) | 0.871 ( 0.186) | 1.010 ( 0.335) | 2.58- 1.75 | 9 | 0.809 ( 0.097) | 0.838 ( 0.170) | 0.691 ( 0.134) | 1.75- 1.45 | 9 | 0.889 ( 0.116) | 0.884 ( 0.166) | 0.864 ( 0.310) | 1.45- 1.35 | 9 | 0.937 ( 0.082) | 0.973 ( 0.123) | 0.854 ( 0.317) | 1.30- 1.06 | 9 | 0.979 ( 0.101) | 1.004 ( 0.152) | 0.890 ( 0.272) | 1.06- 0.88 | 9 | 0.999 ( 0.071) | 0.989 ( 0.128) | 1.077 ( 0.297) | 0.88- 0.79 | 9 | 1.011 ( 0.059) | 1.017 ( 0.117) | 1.043 ( 0.363) | 0.79- 0.73 | 9 | 1.008 ( 0.044) | 0.978 ( 0.143) | 1.136 ( 0.519) | 0.72- 0.68 | 9 | 0.991 ( 0.033) | 0.900 ( 0.068) | 1.084 ( 0.494) | 0.68- 0.63 | 5 | 0.920 ( 0.033) | 0.835 ( 0.031) | 1.120 ( 0.325) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.13- 0.63 | 86 | 0.941 ( 0.109) | 0.933 ( 0.154) | 0.970 ( 0.379) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.0 | 129 | 0.989 ( 0.040) | 1.034 ( 0.067) | 1.111 ( 0.470) | 10.1-14.8 | 129 | 0.993 ( 0.046) | 1.048 ( 0.068) | 1.108 ( 0.531) | 14.8-18.9 | 129 | 0.997 ( 0.187) | 1.036 ( 0.100) | 1.127 ( 0.989) | 18.9-23.4 | 129 | 0.972 ( 0.062) | 1.015 ( 0.085) | 0.939 ( 0.413) | 23.4-27.3 | 129 | 0.967 ( 0.066) | 0.998 ( 0.096) | 0.995 ( 0.461) | 27.3-32.2 | 129 | 0.941 ( 0.081) | 0.961 ( 0.106) | 0.933 ( 0.436) | 32.2-36.3 | 129 | 0.927 ( 0.154) | 0.915 ( 0.136) | 1.077 ( 0.661) | 36.3-38.9 | 129 | 0.884 ( 0.104) | 0.878 ( 0.253) | 1.029 ( 0.487) | 38.9-42.0 | 129 | 0.900 ( 0.096) | 0.847 ( 0.130) | 1.006 ( 0.452) | 42.0-50.1 | 129 | 0.866 ( 0.123) | 0.800 ( 0.143) | 0.914 ( 0.422) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1290 | 0.944 ( 0.115) | 0.953 ( 0.154) | 1.024 ( 0.563) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.14 e2 dimension: a=-0.0069 b=1.24 e3 dimension: a=0.0005 b=1.09 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 4496 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 14:31:22 2019 PROFFITMAIN - Started at Wed Aug 21 14:31:22 2019 OTKP changes: 993 2 5 6 OTKP changes: 993 2 5 6 OTKP changes: 993 2 5 6 No constraint UB - matrix: 0.066087 0.015021 0.006724 ( 0.000014 0.000016 0.000014 ) -0.016083 0.064758 0.013137 ( 0.000013 0.000015 0.000014 ) -0.003753 -0.014354 0.066594 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004640 0.000005 -0.000017 ( 0.000002 0.000001 0.000001 ) 0.000005 0.004625 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000017 -0.000004 0.004653 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066087 0.015021 0.006724 ( 0.000014 0.000016 0.000014 ) -0.016083 0.064758 0.013137 ( 0.000013 0.000015 0.000014 ) -0.003753 -0.014354 0.066594 ( 0.000015 0.000017 0.000016 ) M - matrix: 0.004640 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004640 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004640 ( 0.000000 0.000000 0.000001 ) UB fit with 1015 obs out of 1290 (total:1290,skipped:0) (78.68%) unit cell: 10.413(2) 10.429(2) 10.399(2) 89.949(18) 89.792(18) 90.062(17) V = 1129.3(4) unit cell: 10.4136(7) 10.4136(7) 10.4136(7) 90.0 90.0 90.0 V = 1129.29(14) *** 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 186 obs out of 218 (total:218,skipped:0) (85.32%) UB - matrix: 0.066497 0.011700 0.008959 ( 0.000033 0.000044 0.000036 ) -0.013695 0.065052 0.013248 ( 0.000031 0.000041 0.000034 ) -0.006070 -0.013950 0.065934 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004646 -0.000028 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000028 0.004563 0.000047 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000047 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.501(6) 10.455(6) 90.59(5) 90.18(4) 89.65(4) V = 1142(1) OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 OTKP changes: 188 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066496 0.011700 0.008959 ( 0.000033 0.000043 0.000035 ) -0.013710 0.065040 0.013254 ( 0.000032 0.000042 0.000035 ) -0.006064 -0.013951 0.065940 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004646 -0.000029 0.000014 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000047 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000047 0.004604 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066496 0.011700 0.008959 ( 0.000033 0.000043 0.000035 ) -0.013710 0.065040 0.013254 ( 0.000032 0.000042 0.000035 ) -0.006064 -0.013951 0.065940 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000002 ) UB fit with 188 obs out of 218 (total:218,skipped:0) (86.24%) unit cell: 10.406(5) 10.503(6) 10.454(6) 90.59(5) 90.18(4) 89.64(4) V = 1142(1) unit cell: 10.4539(19) 10.4539(19) 10.4539(19) 90.0 90.0 90.0 V = 1142.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 201 obs out of 218 (total:218,skipped:0) (92.20%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068137 -0.000281 0.000130 ( 0.000028 0.000036 0.000029 ) -0.000048 0.067615 0.000617 ( 0.000031 0.000040 0.000032 ) -0.000028 -0.000052 0.067946 ( 0.000024 0.000030 0.000024 ) M - matrix: 0.004643 -0.000022 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000022 0.004572 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068137 -0.000281 0.000130 ( 0.000028 0.000036 0.000029 ) -0.000048 0.067615 0.000617 ( 0.000031 0.000040 0.000032 ) -0.000028 -0.000052 0.067946 ( 0.000024 0.000030 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 204 obs out of 218 (total:218,skipped:0) (93.58%) unit cell: 10.410(4) 10.491(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1140.0(9) unit cell: 10.4464(13) 10.4464(13) 10.4464(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.066336 0.014186 0.006779 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064704 0.012861 ( 0.000017 0.000022 0.000023 ) -0.004076 -0.014197 0.066901 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.393(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4047(5) 10.4047(5) 10.4047(5) 90.0 90.0 90.0 V = 1126.40(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) UB - matrix: 0.065869 0.015187 0.006797 ( 0.000019 0.000013 0.000019 ) -0.016069 0.064756 0.013249 ( 0.000016 0.000011 0.000016 ) -0.003650 -0.014501 0.066483 ( 0.000021 0.000014 0.000020 ) M - matrix: 0.004610 0.000013 -0.000008 ( 0.000003 0.000001 0.000002 ) 0.000013 0.004634 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000008 -0.000003 0.004642 ( 0.000002 0.000001 0.000003 ) unit cell: 10.447(3) 10.4193(19) 10.411(3) 89.964(19) 89.90(2) 90.158(18) V = 1133.2(5) OTKP changes: 238 1 1 1 OTKP changes: 238 1 1 1 OTKP changes: 238 1 1 1 No constraint UB - matrix: 0.065872 0.015184 0.006797 ( 0.000019 0.000013 0.000019 ) -0.016084 0.064783 0.013255 ( 0.000017 0.000011 0.000016 ) -0.003656 -0.014465 0.066501 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004611 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004637 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004644 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065872 0.015184 0.006797 ( 0.000019 0.000013 0.000019 ) -0.016084 0.064783 0.013255 ( 0.000017 0.000011 0.000016 ) -0.003656 -0.014465 0.066501 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004635 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004635 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004635 ( 0.000000 0.000000 0.000000 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 10.445(3) 10.4168(19) 10.408(3) 89.999(18) 89.89(2) 90.138(18) V = 1132.5(5) unit cell: 10.4234(5) 10.4234(5) 10.4234(5) 90.0 90.0 90.0 V = 1132.46(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.115) HKL list info: 1274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065872 0.015184 0.006797 ( 0.000019 0.000013 0.000019 ) -0.016084 0.064783 0.013255 ( 0.000017 0.000011 0.000016 ) -0.003656 -0.014465 0.066501 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004611 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004637 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004644 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065872 0.015184 0.006797 ( 0.000019 0.000013 0.000019 ) -0.016084 0.064783 0.013255 ( 0.000017 0.000011 0.000016 ) -0.003656 -0.014465 0.066501 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004635 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004635 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004635 ( 0.000000 0.000000 0.000000 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 10.445(3) 10.4168(19) 10.408(3) 89.999(18) 89.89(2) 90.138(18) V = 1132.5(5) unit cell: 10.4234(5) 10.4234(5) 10.4234(5) 90.0 90.0 90.0 V = 1132.46(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 238 obs out of 238 (total:238,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) ******* No constraint UB - matrix: 0.065872 0.015184 0.006797 ( 0.000019 0.000013 0.000019 ) -0.016084 0.064783 0.013255 ( 0.000017 0.000011 0.000016 ) -0.003656 -0.014465 0.066501 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004611 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004637 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004644 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065872 0.015184 0.006797 ( 0.000019 0.000013 0.000019 ) -0.016084 0.064783 0.013255 ( 0.000017 0.000011 0.000016 ) -0.003656 -0.014465 0.066501 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004635 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004635 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004635 ( 0.000000 0.000000 0.000000 ) UB fit with 238 obs out of 238 (total:238,skipped:0) (100.00%) unit cell: 10.445(3) 10.4168(19) 10.408(3) 89.999(18) 89.89(2) 90.138(18) V = 1132.5(5) unit cell: 10.4234(5) 10.4234(5) 10.4234(5) 90.0 90.0 90.0 V = 1132.46(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066096 0.015235 0.006578 ( 0.000014 0.000019 0.000016 ) -0.016350 0.064721 0.012936 ( 0.000012 0.000016 0.000013 ) -0.003369 -0.014191 0.066494 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004647 -0.000003 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 0.004622 -0.000006 ( 0.000002 0.000002 0.000001 ) -0.000001 -0.000006 0.004632 ( 0.000001 0.000001 0.000002 ) unit cell: 10.405(2) 10.433(2) 10.4218(18) 89.923(16) 89.991(16) 89.958(18) V = 1131.3(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066090 0.015226 0.006541 ( 0.000013 0.000018 0.000015 ) -0.016333 0.064725 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003361 -0.014171 0.066539 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004646 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004622 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004638 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066090 0.015226 0.006541 ( 0.000013 0.000018 0.000015 ) -0.016333 0.064725 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003361 -0.014171 0.066539 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004637 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004637 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004637 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.406(2) 10.433(2) 10.4149(18) 89.947(16) 89.962(16) 89.961(18) V = 1130.7(4) unit cell: 10.4181(5) 10.4181(5) 10.4181(5) 90.0 90.0 90.0 V = 1130.74(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.115) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066090 0.015226 0.006541 ( 0.000013 0.000018 0.000015 ) -0.016333 0.064725 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003361 -0.014171 0.066539 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004646 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004622 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004638 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066090 0.015226 0.006541 ( 0.000013 0.000018 0.000015 ) -0.016333 0.064725 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003361 -0.014171 0.066539 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004637 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004637 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004637 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.406(2) 10.433(2) 10.4149(18) 89.947(16) 89.962(16) 89.961(18) V = 1130.7(4) unit cell: 10.4181(5) 10.4181(5) 10.4181(5) 90.0 90.0 90.0 V = 1130.74(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068146 -0.000044 -0.000034 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068000 -0.000050 ( 0.000013 0.000018 0.000015 ) 0.000007 0.000009 0.068105 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004644 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004624 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004638 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068146 -0.000044 -0.000034 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068000 -0.000050 ( 0.000013 0.000018 0.000015 ) 0.000007 0.000009 0.068105 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004637 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004637 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004637 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.4085(16) 10.431(3) 10.4148(15) 89.965(16) 89.977(13) 89.964(17) V = 1130.7(4) unit cell: 10.4180(5) 10.4180(5) 10.4180(5) 90.0 90.0 90.0 V = 1130.72(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 250 obs out of 272 (total:272,skipped:0) (91.91%) UB - matrix: 0.065949 0.015331 0.006322 ( 0.000017 0.000013 0.000013 ) -0.016355 0.064782 0.013397 ( 0.000022 0.000016 0.000016 ) -0.003154 -0.014521 0.066466 ( 0.000031 0.000023 0.000023 ) M - matrix: 0.004627 -0.000003 -0.000012 ( 0.000002 0.000002 0.000002 ) -0.000003 0.004643 -0.000000 ( 0.000002 0.000002 0.000002 ) -0.000012 -0.000000 0.004637 ( 0.000002 0.000002 0.000003 ) unit cell: 10.428(3) 10.410(3) 10.416(3) 90.00(2) 89.85(3) 89.97(2) V = 1130.7(5) OTKP changes: 271 1 1 1 OTKP changes: 271 1 1 1 OTKP changes: 271 1 1 1 No constraint UB - matrix: 0.065984 0.015356 0.006308 ( 0.000016 0.000012 0.000013 ) -0.016357 0.064779 0.013391 ( 0.000018 0.000013 0.000014 ) -0.002858 -0.014639 0.066491 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004630 -0.000005 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004646 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004640 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065984 0.015356 0.006308 ( 0.000016 0.000012 0.000013 ) -0.016357 0.064779 0.013391 ( 0.000018 0.000013 0.000014 ) -0.002858 -0.014639 0.066491 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004636 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004636 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004636 ( 0.000000 0.000000 0.000000 ) UB fit with 271 obs out of 272 (total:272,skipped:0) (99.63%) unit cell: 10.425(2) 10.406(2) 10.4127(18) 89.889(15) 90.088(17) 89.944(18) V = 1129.5(4) unit cell: 10.4144(5) 10.4144(5) 10.4144(5) 90.0 90.0 90.0 V = 1129.53(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.115) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065984 0.015356 0.006308 ( 0.000016 0.000012 0.000013 ) -0.016357 0.064779 0.013391 ( 0.000018 0.000013 0.000014 ) -0.002858 -0.014639 0.066491 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004630 -0.000005 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004646 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004640 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065984 0.015356 0.006308 ( 0.000016 0.000012 0.000013 ) -0.016357 0.064779 0.013391 ( 0.000018 0.000013 0.000014 ) -0.002858 -0.014639 0.066491 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004636 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004636 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004636 ( 0.000000 0.000000 0.000000 ) UB fit with 271 obs out of 272 (total:272,skipped:0) (99.63%) unit cell: 10.425(2) 10.406(2) 10.4127(18) 89.889(15) 90.088(17) 89.944(18) V = 1129.5(4) unit cell: 10.4144(5) 10.4144(5) 10.4144(5) 90.0 90.0 90.0 V = 1129.53(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 271 obs out of 272 (total:272,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068053 -0.000093 0.000069 ( 0.000017 0.000013 0.000013 ) 0.000056 0.068132 -0.000089 ( 0.000014 0.000010 0.000011 ) -0.000016 0.000008 0.068110 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004631 -0.000003 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004642 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004639 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068053 -0.000093 0.000069 ( 0.000017 0.000013 0.000013 ) 0.000056 0.068132 -0.000089 ( 0.000014 0.000010 0.000011 ) -0.000016 0.000008 0.068110 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004636 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004636 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004636 ( 0.000000 0.000000 0.000000 ) UB fit with 271 obs out of 272 (total:272,skipped:0) (99.63%) unit cell: 10.423(3) 10.4106(16) 10.4140(18) 89.932(13) 90.045(17) 89.969(16) V = 1130.0(4) unit cell: 10.4158(5) 10.4158(5) 10.4158(5) 90.0 90.0 90.0 V = 1130.00(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 86 obs out of 86 (total:86,skipped:0) (100.00%) UB - matrix: 0.066195 0.015477 0.006328 ( 0.000025 0.000036 0.000023 ) -0.016452 0.064881 0.012924 ( 0.000035 0.000050 0.000032 ) -0.002996 -0.014217 0.066733 ( 0.000020 0.000029 0.000019 ) M - matrix: 0.004661 -0.000000 0.000006 ( 0.000003 0.000003 0.000002 ) -0.000000 0.004651 -0.000012 ( 0.000003 0.000007 0.000003 ) 0.000006 -0.000012 0.004660 ( 0.000002 0.000003 0.000003 ) unit cell: 10.389(4) 10.400(7) 10.390(3) 89.85(4) 90.08(3) 90.00(4) V = 1122.7(9) OTKP changes: 86 1 1 1 OTKP changes: 86 1 1 1 OTKP changes: 86 1 1 1 OTKP changes: 86 1 1 1 OTKP changes: 86 1 1 1 OTKP changes: 86 1 1 1 Run 6 Omega scan: (-99.000 - -49.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=52.904) HKL list info: 728 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: 0.066195 0.015477 0.006328 ( 0.000025 0.000036 0.000023 ) -0.016452 0.064881 0.012924 ( 0.000035 0.000050 0.000032 ) -0.002996 -0.014217 0.066733 ( 0.000020 0.000029 0.000019 ) M - matrix: 0.004661 -0.000000 0.000006 ( 0.000003 0.000003 0.000002 ) -0.000000 0.004651 -0.000012 ( 0.000003 0.000007 0.000003 ) 0.000006 -0.000012 0.004660 ( 0.000002 0.000003 0.000003 ) Constraint UB - matrix: 0.066195 0.015477 0.006328 ( 0.000025 0.000036 0.000023 ) -0.016452 0.064881 0.012924 ( 0.000035 0.000050 0.000032 ) -0.002996 -0.014217 0.066733 ( 0.000020 0.000029 0.000019 ) M - matrix: 0.004658 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004658 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004658 ( 0.000000 0.000000 0.000001 ) UB fit with 86 obs out of 86 (total:86,skipped:0) (100.00%) unit cell: 10.389(4) 10.400(7) 10.390(3) 89.85(4) 90.08(3) 90.00(4) V = 1122.7(9) unit cell: 10.3932(9) 10.3932(9) 10.3932(9) 90.0 90.0 90.0 V = 1122.66(17) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_26.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068138 0.000019 -0.000066 ( 0.000009 0.000010 0.000009 ) -0.000002 0.068041 0.000008 ( 0.000010 0.000010 0.000010 ) 0.000032 -0.000020 0.068137 ( 0.000007 0.000008 0.000008 ) M - matrix: 0.004643 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.004630 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000001 0.004643 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068138 0.000019 -0.000066 ( 0.000009 0.000010 0.000009 ) -0.000002 0.068041 0.000008 ( 0.000010 0.000010 0.000010 ) 0.000032 -0.000020 0.068137 ( 0.000007 0.000008 0.000008 ) M - matrix: 0.004639 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004639 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004639 ( 0.000000 0.000000 0.000000 ) UB fit with 1268 obs out of 1290 (total:1290,skipped:0) (98.29%) unit cell: 10.4097(14) 10.4245(16) 10.4100(11) 89.990(11) 89.971(10) 90.014(11) V = 1129.7(3) unit cell: 10.4147(4) 10.4147(4) 10.4147(4) 90.0 90.0 90.0 V = 1129.65(7) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 127 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof 5664 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:31:31 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.115) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.115) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.115) Run 6 Omega scan: (-99.000 - -49.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=52.904) PROFFIT INFO: signal sum: min=-762.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-680.4858 max=1270247.8547 PROFFIT INFO: background sum: min=-190.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=401.0000 max=6068.0000 PROFFIT INFO: num of signal pixels: min=42 max=533 PROFFIT INFO: Inet: min=-1088.7773 max=2032396.6250 PROFFIT INFO: sig(Inet): min=52.0012 max=30699.6230 PROFFIT INFO: Inet/sig(Inet): min=-2.04 max=247.34 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 490 1939 2929 3506 3786 4395 4778 5014 5367 5604 5664 Percent 8.7 34.2 51.7 61.9 66.8 77.6 84.4 88.5 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5664 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 5664 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2032397- 129106 566 417225.77 77.20 100.00 128918- 4051 566 28572.19 19.44 100.00 4042- 2060 566 2893.80 7.18 97.00 2058- 1247 566 1598.70 3.86 52.12 1246- 828 566 1014.53 2.37 16.61 827- 548 566 678.63 1.76 9.19 548- 342 566 438.38 1.23 5.30 342- 154 566 247.07 0.72 1.06 153- 19 566 81.81 0.29 0.00 19- -1089 570 -127.77 -0.25 0.00 ------------------------------------------------------------------------------------ 2032397- -1089 5664 45230.26 11.37 38.10 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 566 114009.61 15.69 68.90 1.73- 1.26 566 86123.76 20.72 60.07 1.26- 1.09 566 60972.63 18.60 66.43 1.09- 0.97 566 54914.57 14.91 34.81 0.97- 0.88 566 17701.39 7.13 44.35 0.88- 0.80 566 50392.09 14.16 36.22 0.80- 0.76 566 18768.74 5.84 19.08 0.76- 0.71 566 21150.37 6.84 16.25 0.71- 0.67 566 24943.87 8.12 28.80 0.67- 0.63 570 3619.60 1.79 6.32 ------------------------------------------------------------------------------------ 6.00- 0.63 5664 45230.26 11.37 38.10 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:31:31 2019 Sorting 5664 observations 53 unique observations with > 7.00 F2/sig(F2) 5664 observations in 6 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 48 564 Total number of frames 564 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 11 frame = 1 scale 5664 observations in 6 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 9 50 6 0 4 55 Total number of frames 55 1363 observations > 7.00 F2/sig(F2) 1363 observations in 6 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 9 50 6 0 4 55 Total number of frames 55 Removing 'redundancy=1' reflections Average redundancy: 20.2 (Out of 1363 removed 7 = 1356, unique = 67) 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 1356 observations in 6 runs Run # start # end # total # 1 0 9 10 2 0 9 20 3 0 9 30 4 0 9 40 5 0 9 50 6 0 4 55 Total number of frames 55 67 unique data precomputed (should be 67) 67 unique data with 1356 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.2 (Out of 1356 removed 0 = 1356, unique = 67) 67 unique data precomputed (should be 67) 67 unique data with 1356 observations RMS deviation of equivalent data = 0.31837 Rint = 0.25569 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24787, wR= 0.34417 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13013, wR= 0.19018, Acormin=0.485, Acormax=1.425, Acor_av=0.997 F test: Probability=1.000, F= 3.614 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11830, wR= 0.17589, Acormin=0.458, Acormax=1.479, Acor_av=0.956 F test: Probability=1.000, F= 1.207 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12019, wR= 0.17901, Acormin=0.517, Acormax=1.538, Acor_av=0.994 F test: Probability=0.000, F= 0.964 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10494, wR= 0.16092, Acormin=0.409, Acormax=1.609, Acor_av=0.955 F test: Probability=1.000, F= 1.262 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09352, wR= 0.14908, Acormin=0.511, Acormax=1.793, Acor_av=0.988 F test: Probability=1.000, F= 1.252 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11499, wR= 0.17046, Acormin=0.409, Acormax=1.617, Acor_av=0.967 F test: Probability=0.000, F= 0.660 Trying model 7 (ne=6, no=1)... Results: Rint= 0.10320, wR= 0.15611, Acormin=0.388, Acormax=1.634, Acor_av=0.943 F test: Probability=0.000, F= 0.817 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09034, wR= 0.14423, Acormin=0.456, Acormax=1.786, Acor_av=0.976 F test: Probability=0.851, F= 1.061 Trying model 9 (ne=6, no=5)... Results: Rint= 0.15052, wR= 0.19149, Acormin=0.025, Acormax=1.036, Acor_av=0.468 F test: Probability=0.000, F= 0.379 Final absorption model (ne=4, no=3): Rint= 0.09352, Acormin=0.511, Acormax=1.793, Acor_av=0.988 Combined refinement in use Rint: 0.25752 There are 55 active scales (one needs to be fixed) Refinement control: frame scale #46 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 78 pars with 3081 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31837 Using Levenberg-Marquardt: 0.00010 New wR= 0.10597 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25569 with corrections 0.07899 Rint for all data: 0.25752 with corrections 0.08173 2 observations identified as outliers and rejected Cycle 2 wR= 0.09678 Using Levenberg-Marquardt: 0.00001 New wR= 0.07930 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25508 with corrections 0.05546 Rint for all data: 0.25752 with corrections 0.06145 1 observations identified as outliers and rejected Cycle 3 wR= 0.07630 Using Levenberg-Marquardt: 0.00000 New wR= 0.07472 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25479 with corrections 0.05266 Rint for all data: 0.25752 with corrections 0.05891 1 observations identified as outliers and rejected Cycle 4 wR= 0.07171 Using Levenberg-Marquardt: 0.00000 New wR= 0.07088 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25427 with corrections 0.05047 Rint for all data: 0.25752 with corrections 0.05710 0 observations identified as outliers and rejected Cycle 5 wR= 0.07088 Using Levenberg-Marquardt: 0.00000 New wR= 0.07027 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25427 with corrections 0.05007 Rint for all data: 0.25752 with corrections 0.05671 0 observations identified as outliers and rejected Final wR= 0.07027 Final frame scales: Min= 0.7726 Max= 1.2919 Final absorption correction factors: Amin= 0.3489 Amax= 1.6194 PROFFIT INFO: Inet (after scale3 abspack): min=-1065.2058 max=1257467.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.5951 max=24041.6211 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/104 5664 reflections read from tmp file 213 reflections are rejected (212 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 3 5 5 3 5 5 7 204 Initial Chi^2= 0.52747 Cycle 1, Chi^2= 1.02114 Current error model SIG(F2)^2 = 64.47*I_RAW + 10.13*I_BACK+(0.03652*)^2 Cycle 2, Chi^2= 1.01648 Current error model SIG(F2)^2 = 78.83*I_RAW + 7.05*I_BACK+(0.02937*)^2 Cycle 3, Chi^2= 1.00840 Current error model SIG(F2)^2 = 85.01*I_RAW + 5.92*I_BACK+(0.02731*)^2 Cycle 4, Chi^2= 1.00329 Current error model SIG(F2)^2 = 87.40*I_RAW + 5.53*I_BACK+(0.02673*)^2 Cycle 5, Chi^2= 1.00114 Current error model SIG(F2)^2 = 88.24*I_RAW + 5.40*I_BACK+(0.02655*)^2 Cycle 6, Chi^2= 1.00038 Current error model SIG(F2)^2 = 88.52*I_RAW + 5.36*I_BACK+(0.02650*)^2 Cycle 7, Chi^2= 1.00012 Current error model SIG(F2)^2 = 88.62*I_RAW + 5.35*I_BACK+(0.02648*)^2 Final Chi^2= 1.00012 Final error model SIG(F2)^2 = 88.62*I_RAW + 5.35*I_BACK+(0.02648*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1257467- 115237 566 379137.14 30.28 100.00 114663- 3441 566 28353.49 12.83 100.00 3440- 2009 566 2664.50 6.08 99.12 2007- 1151 566 1501.29 3.94 64.13 1150- 777 566 947.35 2.74 25.97 776- 514 566 642.42 2.39 16.25 514- 330 566 418.34 1.96 8.66 330- 147 566 239.84 1.47 3.18 146- 19 566 80.76 0.74 0.35 19- -1065 570 -128.21 -0.53 0.00 ------------------------------------------------------------------------------------ 1257467- -1065 5664 41356.37 6.19 41.74 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 566 104765.07 10.11 71.73 1.73- 1.26 566 78740.44 9.31 62.90 1.26- 1.09 566 56472.71 8.15 70.85 1.09- 0.97 566 49676.79 6.53 36.75 0.97- 0.88 566 15610.46 4.74 51.59 0.88- 0.80 566 46758.15 7.38 42.40 0.80- 0.76 566 17262.62 3.83 21.73 0.76- 0.71 566 18781.29 4.73 19.61 0.71- 0.67 566 22387.48 5.40 32.16 0.67- 0.63 570 3377.15 1.70 7.89 ------------------------------------------------------------------------------------ 6.00- 0.63 5664 41356.37 6.19 41.74 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 566 104765.07 10.11 71.73 6.00- 1.26 1132 91752.75 9.71 67.31 6.00- 1.09 1698 79992.74 9.19 68.49 6.00- 0.97 2264 72413.75 8.52 60.56 6.00- 0.88 2830 61053.09 7.77 58.76 6.00- 0.80 3396 58670.60 7.70 56.04 6.00- 0.76 3962 52755.18 7.15 51.14 6.00- 0.71 4528 48508.44 6.85 47.20 6.00- 0.67 5094 45606.11 6.69 45.52 6.00- 0.63 5664 41356.37 6.19 41.74 ------------------------------------------------------------------------------------ 6.00- 0.63 5664 41356.37 6.19 41.74 Scale applied to data: s=0.795249 (maximum obs:1257467.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.057; Rsigma 0.038: data 5664 -> merged 240 With outlier rejection... Rint 0.049; Rsigma 0.038: data 5644 -> merged 240 Rejected total: 20, method kkm 13, method Blessing 7 Completeness direct cell (a, b, c) = (10.415, 10.415, 10.415), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626894, 6.012955 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.40 - 1.59 21 21 31.19 100.00 655 1.57 - 1.20 21 21 32.14 100.00 675 1.19 - 1.02 21 21 29.90 100.00 628 1.02 - 0.91 21 21 28.81 100.00 605 0.91 - 0.84 21 21 25.57 100.00 537 0.84 - 0.79 21 21 25.19 100.00 529 0.78 - 0.74 21 21 23.76 100.00 499 0.74 - 0.71 21 21 19.95 100.00 419 0.71 - 0.68 21 21 22.14 100.00 465 0.68 - 0.65 23 23 18.83 100.00 433 --------------------------------------------------------------- 10.40 - 0.65 212 212 25.68 100.00 5445 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:31:31 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.409746 10.424540 10.409952 89.9901 89.9709 90.0141 5644 Reflections read from file xs2212a.hkl 5608 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.18 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2815 0 3724 3715 5608 N (int>3sigma) = 0 0 0 0 1253 0 1649 1627 2348 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 33.5 31.7 32.5 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.2 6.2 Lattice type: F chosen Volume: 1129.65 ------------------------------------------------------------------------------- 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: 7.359 7.363 7.365 119.99 119.96 90.00 Niggli form: a.a = 54.155 b.b = 54.210 c.c = 54.245 b.c = -27.102 a.c = -27.066 a.b = -0.001 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.090 CUBIC F-lattice R(int) = 0.049 [ 5377] Vol = 1129.7 Cell: 10.425 10.410 10.410 89.97 90.01 89.99 Volume: 1129.65 Matrix: 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.109 TETRAGONAL I-lattice R(int) = 0.048 [ 4992] Vol = 564.8 Cell: 7.365 7.367 10.410 90.01 89.97 89.92 Volume: 564.83 Matrix: 0.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.062 TETRAGONAL I-lattice R(int) = 0.048 [ 4993] Vol = 564.8 Cell: 7.359 7.363 10.425 90.00 89.98 90.00 Volume: 564.83 Matrix: 0.5000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.089 TETRAGONAL I-lattice R(int) = 0.048 [ 4992] Vol = 564.8 Cell: 7.367 7.365 10.410 90.03 90.01 90.08 Volume: 564.83 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.066 ORTHORHOMBIC F-lattice R(int) = 0.048 [ 4939] Vol = 1129.7 Cell: 10.410 10.410 10.425 89.99 90.01 89.97 Volume: 1129.65 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.122 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4915] Vol = 564.8 Cell: 10.410 7.367 7.365 89.92 89.97 90.01 Volume: 564.83 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [42] err= 0.012 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 4921] Vol = 564.8 Cell: 7.359 7.363 10.425 90.00 90.02 90.00 Volume: 564.83 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.063 MONOCLINIC I-lattice R(int) = 0.046 [ 4393] Vol = 564.8 Cell: 7.365 10.410 7.367 90.01 90.08 90.03 Volume: 564.83 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [14] err= 0.061 MONOCLINIC I-lattice R(int) = 0.045 [ 4394] Vol = 564.8 Cell: 7.365 10.410 7.367 89.99 90.08 89.97 Volume: 564.83 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.057 MONOCLINIC I-lattice R(int) = 0.046 [ 4393] Vol = 564.8 Cell: 7.367 10.410 7.365 90.03 90.08 90.01 Volume: 564.83 Matrix: 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [37] err= 0.012 MONOCLINIC I-lattice R(int) = 0.044 [ 4373] Vol = 564.8 Cell: 7.363 7.359 10.425 89.98 90.00 90.00 Volume: 564.83 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.003 MONOCLINIC I-lattice R(int) = 0.044 [ 4383] Vol = 564.8 Cell: 7.359 7.363 10.425 90.00 90.02 90.00 Volume: 564.83 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.012 MONOCLINIC I-lattice R(int) = 0.045 [ 4395] Vol = 564.8 Cell: 7.359 10.425 7.363 90.00 90.00 89.98 Volume: 564.83 Matrix:-0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.032 MONOCLINIC I-lattice R(int) = 0.045 [ 4395] Vol = 564.8 Cell: 7.359 10.425 7.363 90.00 90.00 90.02 Volume: 564.83 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 [ 3338] Vol = 282.4 Cell: 7.359 7.363 7.365 119.99 119.96 90.00 Volume: 282.41 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 2815 0 3715 3727 5608 N (int>3sigma) = 0 0 0 0 1253 0 1627 1651 2348 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 31.7 33.5 32.5 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.2 6.3 6.2 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.520 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 39 39 412 1108 N I>3s 2 2 2 593 0.0 0.0 0.0 2.0 0.9 0.9 0.3 5.0 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 0.049 4993 Fd-3m 1 1 227 C N N N N 37 2284 0.049 5055 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.424540 10.409952 10.409746 89.9709 90.0141 89.9901 ZERR 5.00 0.001585 0.001149 0.001362 0.0099 0.0114 0.0107 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1144301- 127365 558 548 26 21.1 380654.99 30.35 0.044 0.057 108225- 3166 645 642 26 24.7 26661.92 12.10 0.067 0.078 2966- 1394 822 818 26 31.5 2203.42 5.53 0.130 0.186 1351- 870 711 711 26 27.3 1046.63 2.75 0.233 0.302 847- 482 705 705 26 27.1 644.13 2.41 0.297 0.402 477- 305 668 668 26 25.7 379.20 1.63 0.448 0.620 297- 144 559 559 26 21.5 224.24 1.30 0.576 0.872 142- 33 511 510 26 19.6 73.40 0.55 0.880 2.364 24- -216 485 483 32 15.1 -21.51 -0.03 0.991 5.596 ------------------------------------------------------------------------------------------- 1144301- -216 5664 5644 240 23.5 40595.72 6.14 0.049 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-1.44 839 834 26 32.1 112929.65 11.02 0.042 0.051 0.029 1.39-1.09 865 863 26 33.2 43312.88 7.18 0.047 0.063 0.035 1.06-0.94 721 719 26 27.7 38895.03 5.65 0.047 0.055 0.037 0.92-0.84 684 682 26 26.2 41869.86 7.38 0.052 0.067 0.042 0.84-0.78 667 665 26 25.6 24146.17 4.94 0.059 0.077 0.048 0.78-0.73 570 570 26 21.9 8292.62 3.02 0.082 0.096 0.077 0.73-0.69 567 565 26 21.7 19810.85 4.76 0.065 0.078 0.061 0.69-0.66 544 542 28 19.4 13796.73 3.72 0.079 0.107 0.069 0.65-0.63 207 204 30 6.8 7765.61 2.33 0.079 0.080 0.088 ------------------------------------------------------------------------------------------------------ inf-0.63 5664 5644 240 23.5 40595.72 6.14 0.049 0.063 0.038 inf-0.65 5461 5443 211 25.8 41852.02 6.29 0.049 0.062 0.038 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-1.44 834 26 26 100.0 32.1 112929.65 62.77 0.042 0.007 1.39-1.09 863 26 26 100.0 33.2 43312.88 37.53 0.047 0.008 1.06-0.94 719 26 26 100.0 27.7 38895.03 30.86 0.047 0.008 0.92-0.84 682 26 26 100.0 26.2 41869.86 37.44 0.052 0.009 0.84-0.78 665 26 26 100.0 25.6 24146.17 23.78 0.059 0.010 0.78-0.73 570 26 26 100.0 21.9 8292.62 14.17 0.082 0.017 0.73-0.69 565 26 26 100.0 21.7 19810.85 21.17 0.065 0.014 0.69-0.66 542 28 28 100.0 19.4 13796.73 17.74 0.079 0.016 0.65-0.63 204 30 30 100.0 6.8 7765.61 5.82 0.079 0.037 -------------------------------------------------------------------------------------------- inf-0.63 5644 240 240 100.0 23.5 40595.72 31.74 0.049 0.009 inf-0.65 5443 211 211 100.0 25.8 41852.02 32.71 0.049 0.009 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066110 0.014970 0.006887 ( 0.000009 0.000009 0.000009 ) -0.016082 0.064794 0.013180 ( 0.000010 0.000010 0.000010 ) -0.003691 -0.014396 0.066494 ( 0.000007 0.000008 0.000008 ) M - matrix: 0.004643 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.004630 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000000 0.004643 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066110 0.014970 0.006887 ( 0.000009 0.000009 0.000009 ) -0.016082 0.064794 0.013180 ( 0.000010 0.000010 0.000010 ) -0.003691 -0.014396 0.066494 ( 0.000007 0.000008 0.000008 ) M - matrix: 0.004639 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004639 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004639 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4097(13) 10.4245(16) 10.4099(11) 89.998(11) 89.974(10) 90.010(11) V = 1129.6(3) unit cell: 10.4147(4) 10.4147(4) 10.4147(4) 90.0 90.0 90.0 V = 1129.65(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.115) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.115) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.115) Run 6 Omega scan: (-99.000 - -49.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=52.904) PROFFIT INFO: signal sum: min=-762.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-680.4858 max=1270247.8547 PROFFIT INFO: background sum: min=-190.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=401.0000 max=6068.0000 PROFFIT INFO: num of signal pixels: min=42 max=533 PROFFIT INFO: Inet: min=-1088.7773 max=2032396.6250 PROFFIT INFO: sig(Inet): min=52.0012 max=30699.6230 PROFFIT INFO: Inet/sig(Inet): min=-2.04 max=247.34 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 980 3878 5858 7012 7572 8790 9556 10028 10734 11208 11328 Percent 8.7 34.2 51.7 61.9 66.8 77.6 84.4 88.5 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5664 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 5664 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2032397- 129106 566 417225.77 77.20 100.00 128918- 4051 566 28572.19 19.44 100.00 4042- 2060 566 2893.80 7.18 97.00 2058- 1247 566 1598.70 3.86 52.12 1246- 828 566 1014.53 2.37 16.61 827- 548 566 678.63 1.76 9.19 548- 342 566 438.38 1.23 5.30 342- 154 566 247.07 0.72 1.06 153- 19 566 81.81 0.29 0.00 19- -1089 570 -127.77 -0.25 0.00 ------------------------------------------------------------------------------------ 2032397- -1089 5664 45230.26 11.37 38.10 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 566 114009.61 15.69 68.90 1.73- 1.26 566 86123.76 20.72 60.07 1.26- 1.09 566 60972.63 18.60 66.43 1.09- 0.97 566 54914.57 14.91 34.81 0.97- 0.88 566 17701.39 7.13 44.35 0.88- 0.80 566 50392.09 14.16 36.22 0.80- 0.76 566 18768.74 5.84 19.08 0.76- 0.71 566 21150.37 6.84 16.25 0.71- 0.67 566 24943.87 8.12 28.80 0.67- 0.63 570 3619.60 1.79 6.32 ------------------------------------------------------------------------------------ 6.00- 0.63 5664 45230.26 11.37 38.10 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:31:32 2019 Sorting 5664 observations 43 unique observations with > 7.00 F2/sig(F2) 5664 observations in 6 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 48 564 Total number of frames 564 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 14 frame = 1 scale 5664 observations in 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 3 44 Total number of frames 44 1363 observations > 7.00 F2/sig(F2) 1363 observations in 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 3 44 Total number of frames 44 Removing 'redundancy=1' reflections Average redundancy: 24.7 (Out of 1363 removed 3 = 1360, unique = 55) 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 1360 observations in 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 3 44 Total number of frames 44 55 unique data precomputed (should be 55) 55 unique data with 1360 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 24.7 (Out of 1360 removed 0 = 1360, unique = 55) 55 unique data precomputed (should be 55) 55 unique data with 1360 observations RMS deviation of equivalent data = 0.31880 Rint = 0.25592 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24811, wR= 0.34458 Trying model 1 (ne=2, no=0)... Results: Rint= 0.12999, wR= 0.19076, Acormin=0.485, Acormax=1.424, Acor_av=0.997 F test: Probability=1.000, F= 3.629 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11837, wR= 0.17660, Acormin=0.458, Acormax=1.478, Acor_av=0.956 F test: Probability=1.000, F= 1.203 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11951, wR= 0.17989, Acormin=0.517, Acormax=1.539, Acor_av=0.995 F test: Probability=0.000, F= 0.976 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10517, wR= 0.16169, Acormin=0.411, Acormax=1.610, Acor_av=0.955 F test: Probability=1.000, F= 1.258 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09352, wR= 0.14978, Acormin=0.515, Acormax=1.799, Acor_av=0.989 F test: Probability=1.000, F= 1.258 Final absorption model (ne=4, no=3): Rint= 0.09352, Acormin=0.515, Acormax=1.799, Acor_av=0.989 Combined refinement in use Rint: 0.25777 There are 44 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 67 pars with 2278 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31880 Using Levenberg-Marquardt: 0.00010 New wR= 0.12251 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25592 with corrections 0.08995 Rint for all data: 0.25777 with corrections 0.09261 6 observations identified as outliers and rejected Cycle 2 wR= 0.10247 Using Levenberg-Marquardt: 0.00001 New wR= 0.07883 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25440 with corrections 0.05729 Rint for all data: 0.25777 with corrections 0.06465 0 observations identified as outliers and rejected Cycle 3 wR= 0.07883 Using Levenberg-Marquardt: 0.00000 New wR= 0.07522 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25440 with corrections 0.05298 Rint for all data: 0.25777 with corrections 0.05968 0 observations identified as outliers and rejected Cycle 4 wR= 0.07522 Using Levenberg-Marquardt: 0.00000 New wR= 0.07327 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25440 with corrections 0.05149 Rint for all data: 0.25777 with corrections 0.05808 0 observations identified as outliers and rejected Cycle 5 wR= 0.07327 Using Levenberg-Marquardt: 0.00000 New wR= 0.07254 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25440 with corrections 0.05054 Rint for all data: 0.25777 with corrections 0.05698 1 observations identified as outliers and rejected Final wR= 0.07254 Final frame scales: Min= 0.6899 Max= 1.2536 Final absorption correction factors: Amin= 0.3620 Amax= 1.5898 PROFFIT INFO: Inet (after scale3 abspack): min=-1031.6576 max=1232754.6250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.0149 max=23853.0371 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/104 5664 reflections read from tmp file 233 reflections are rejected (233 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 1 6 3 0 3 1 3 145 Initial Chi^2= 0.52134 Cycle 1, Chi^2= 1.00510 Current error model SIG(F2)^2 = 62.09*I_RAW + 11.37*I_BACK+(0.03698*)^2 Cycle 2, Chi^2= 1.01612 Current error model SIG(F2)^2 = 78.22*I_RAW + 7.28*I_BACK+(0.02896*)^2 Cycle 3, Chi^2= 1.00910 Current error model SIG(F2)^2 = 85.15*I_RAW + 5.87*I_BACK+(0.02699*)^2 Cycle 4, Chi^2= 1.00313 Current error model SIG(F2)^2 = 87.49*I_RAW + 5.46*I_BACK+(0.02667*)^2 Cycle 5, Chi^2= 1.00094 Current error model SIG(F2)^2 = 88.20*I_RAW + 5.35*I_BACK+(0.02661*)^2 Cycle 6, Chi^2= 1.00028 Current error model SIG(F2)^2 = 88.41*I_RAW + 5.31*I_BACK+(0.02659*)^2 Cycle 7, Chi^2= 1.00008 Current error model SIG(F2)^2 = 88.47*I_RAW + 5.30*I_BACK+(0.02659*)^2 Final Chi^2= 1.00008 Final error model SIG(F2)^2 = 88.47*I_RAW + 5.30*I_BACK+(0.02659*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1232755- 115404 566 378415.96 30.21 100.00 115385- 3462 566 28252.81 12.82 100.00 3446- 2021 566 2659.71 6.13 99.12 2020- 1149 566 1507.52 3.90 64.31 1147- 775 566 946.37 2.76 25.44 774- 514 566 641.32 2.39 16.61 513- 329 566 417.51 1.96 9.01 329- 147 566 239.60 1.47 3.00 147- 19 566 80.58 0.74 0.53 19- -1032 570 -127.89 -0.53 0.00 ------------------------------------------------------------------------------------ 1232755- -1032 5664 41274.09 6.18 41.77 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 566 104430.08 10.09 71.73 1.73- 1.26 566 78682.19 9.28 63.25 1.26- 1.09 566 56349.95 8.14 70.85 1.09- 0.97 566 49349.05 6.53 36.75 0.97- 0.88 566 15691.13 4.74 51.59 0.88- 0.80 566 46696.38 7.39 42.40 0.80- 0.76 566 17276.12 3.83 21.73 0.76- 0.71 566 18799.49 4.73 19.61 0.71- 0.67 566 22381.67 5.41 32.16 0.67- 0.63 570 3352.81 1.70 7.89 ------------------------------------------------------------------------------------ 6.00- 0.63 5664 41274.09 6.18 41.77 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 566 104430.08 10.09 71.73 6.00- 1.26 1132 91556.13 9.69 67.49 6.00- 1.09 1698 79820.74 9.17 68.61 6.00- 0.97 2264 72202.82 8.51 60.64 6.00- 0.88 2830 60900.48 7.76 58.83 6.00- 0.80 3396 58533.13 7.69 56.10 6.00- 0.76 3962 52639.27 7.14 51.19 6.00- 0.71 4528 48409.30 6.84 47.24 6.00- 0.67 5094 45517.34 6.68 45.56 6.00- 0.63 5664 41274.09 6.18 41.77 ------------------------------------------------------------------------------------ 6.00- 0.63 5664 41274.09 6.18 41.77 Scale applied to data: s=0.811191 (maximum obs:1232754.625,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.057; Rsigma 0.038: data 5664 -> merged 162 With outlier rejection... Rint 0.051; Rsigma 0.038: data 5649 -> merged 162 Rejected total: 15, method kkm 6, method Blessing 9 Completeness direct cell (a, b, c) = (10.415, 10.415, 10.415), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626893, 6.012942 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.40 - 1.76 14 14 37.29 100.00 522 1.74 - 1.27 14 14 40.64 100.00 569 1.26 - 1.06 14 14 45.71 100.00 640 1.05 - 0.97 14 14 39.71 100.00 556 0.95 - 0.88 14 14 41.50 100.00 581 0.87 - 0.81 14 14 36.93 100.00 517 0.80 - 0.76 14 14 38.64 100.00 541 0.76 - 0.72 14 14 32.50 100.00 455 0.72 - 0.69 14 14 35.86 100.00 502 0.69 - 0.65 19 19 29.84 100.00 567 --------------------------------------------------------------- 10.40 - 0.65 145 145 37.59 100.00 5450 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:31:31 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.409746 10.424540 10.409952 89.9901 89.9709 90.0141 5644 Reflections read from file xs2212a.hkl 5608 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.18 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2815 0 3724 3715 5608 N (int>3sigma) = 0 0 0 0 1253 0 1649 1627 2348 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 33.5 31.7 32.5 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.2 6.2 Lattice type: F chosen Volume: 1129.65 ------------------------------------------------------------------------------- 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: 7.359 7.363 7.365 119.99 119.96 90.00 Niggli form: a.a = 54.155 b.b = 54.210 c.c = 54.245 b.c = -27.102 a.c = -27.066 a.b = -0.001 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.090 CUBIC F-lattice R(int) = 0.049 [ 5377] Vol = 1129.7 Cell: 10.425 10.410 10.410 89.97 90.01 89.99 Volume: 1129.65 Matrix: 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.109 TETRAGONAL I-lattice R(int) = 0.048 [ 4992] Vol = 564.8 Cell: 7.365 7.367 10.410 90.01 89.97 89.92 Volume: 564.83 Matrix: 0.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.062 TETRAGONAL I-lattice R(int) = 0.048 [ 4993] Vol = 564.8 Cell: 7.359 7.363 10.425 90.00 89.98 90.00 Volume: 564.83 Matrix: 0.5000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.089 TETRAGONAL I-lattice R(int) = 0.048 [ 4992] Vol = 564.8 Cell: 7.367 7.365 10.410 90.03 90.01 90.08 Volume: 564.83 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.066 ORTHORHOMBIC F-lattice R(int) = 0.048 [ 4939] Vol = 1129.7 Cell: 10.410 10.410 10.425 89.99 90.01 89.97 Volume: 1129.65 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.122 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4915] Vol = 564.8 Cell: 10.410 7.367 7.365 89.92 89.97 90.01 Volume: 564.83 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [42] err= 0.012 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 4921] Vol = 564.8 Cell: 7.359 7.363 10.425 90.00 90.02 90.00 Volume: 564.83 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.063 MONOCLINIC I-lattice R(int) = 0.046 [ 4393] Vol = 564.8 Cell: 7.365 10.410 7.367 90.01 90.08 90.03 Volume: 564.83 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [14] err= 0.061 MONOCLINIC I-lattice R(int) = 0.045 [ 4394] Vol = 564.8 Cell: 7.365 10.410 7.367 89.99 90.08 89.97 Volume: 564.83 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.057 MONOCLINIC I-lattice R(int) = 0.046 [ 4393] Vol = 564.8 Cell: 7.367 10.410 7.365 90.03 90.08 90.01 Volume: 564.83 Matrix: 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [37] err= 0.012 MONOCLINIC I-lattice R(int) = 0.044 [ 4373] Vol = 564.8 Cell: 7.363 7.359 10.425 89.98 90.00 90.00 Volume: 564.83 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.003 MONOCLINIC I-lattice R(int) = 0.044 [ 4383] Vol = 564.8 Cell: 7.359 7.363 10.425 90.00 90.02 90.00 Volume: 564.83 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.012 MONOCLINIC I-lattice R(int) = 0.045 [ 4395] Vol = 564.8 Cell: 7.359 10.425 7.363 90.00 90.00 89.98 Volume: 564.83 Matrix:-0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.032 MONOCLINIC I-lattice R(int) = 0.045 [ 4395] Vol = 564.8 Cell: 7.359 10.425 7.363 90.00 90.00 90.02 Volume: 564.83 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 [ 3338] Vol = 282.4 Cell: 7.359 7.363 7.365 119.99 119.96 90.00 Volume: 282.41 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 2815 0 3715 3727 5608 N (int>3sigma) = 0 0 0 0 1253 0 1627 1651 2348 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 31.7 33.5 32.5 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.2 6.3 6.2 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.520 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 39 39 412 1108 N I>3s 2 2 2 593 0.0 0.0 0.0 2.0 0.9 0.9 0.3 5.0 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 0.049 4993 Fd-3m 1 1 227 C N N N N 37 2284 0.049 5055 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.424540 10.409952 10.409746 89.9709 90.0141 89.9901 ZERR 5.00 0.001585 0.001149 0.001362 0.0099 0.0114 0.0107 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1141717- 89833 685 676 27 25.0 329624.16 28.45 0.047 0.058 76604- 1798 1071 1069 27 39.6 5196.50 8.21 0.086 0.095 1660- 781 1144 1142 27 42.3 1119.84 2.94 0.224 0.301 748- 322 1115 1114 27 41.3 490.88 2.02 0.368 0.522 316- 77 804 803 27 29.7 213.44 1.21 0.600 1.050 70- -148 845 845 27 31.3 14.28 0.21 0.966 4.853 ------------------------------------------------------------------------------------------- 1141717- -148 5664 5649 162 34.9 40784.24 6.15 0.051 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-1.27 1092 1089 27 40.3 93303.23 9.93 0.043 0.053 0.030 1.26-0.97 1201 1196 28 42.7 49094.39 6.92 0.048 0.059 0.035 0.95-0.81 1100 1098 28 39.2 32082.38 6.22 0.056 0.074 0.044 0.80-0.73 974 973 27 36.0 17651.07 4.20 0.060 0.075 0.056 0.72-0.67 864 863 27 32.0 18380.99 4.59 0.077 0.103 0.063 0.66-0.63 433 430 25 17.2 4191.37 1.84 0.109 0.086 0.122 ------------------------------------------------------------------------------------------------------ inf-0.63 5664 5649 162 34.9 40784.24 6.15 0.051 0.062 0.038 inf-0.65 5461 5448 144 37.8 42047.30 6.30 0.050 0.061 0.038 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-1.27 1089 27 27 100.0 40.3 93303.23 60.37 0.043 0.007 1.26-0.97 1196 28 28 100.0 42.7 49094.39 42.53 0.048 0.007 0.95-0.81 1098 28 28 100.0 39.2 32082.38 38.79 0.056 0.009 0.80-0.73 973 27 27 100.0 36.0 17651.07 22.83 0.060 0.011 0.72-0.67 863 27 27 100.0 32.0 18380.99 27.77 0.077 0.012 0.66-0.63 430 25 25 100.0 17.2 4191.37 7.59 0.109 0.031 -------------------------------------------------------------------------------------------- inf-0.63 5649 162 162 100.0 34.9 40784.24 36.93 0.051 0.008 inf-0.65 5448 144 144 100.0 37.8 42047.30 38.07 0.050 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:37:56 2019) ID: 3668; threads 40; handles 811; mem 514788.00 (1204692.00)kB; time: 1w 5d 0h 48m 44s MEMORY INFO: Memory PF:219.0, Ph:549.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.7,peak PF: 700.2, WS: 471.1, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:220.0, Ph:551.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.5,peak PF: 700.2, WS: 472.9, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:37:56 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000015 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000014 0.000013 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000016 0.000015 ) 10.42433 ( 0.00228 ) 10.43788 ( 0.00213 ) 10.40727 ( 0.00226 ) 89.88512 ( 0.01720 ) 89.79539 ( 0.01764 ) 90.20497 ( 0.01735 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:37:56 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000015 0.000017 0.000015 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000014 0.000013 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000016 0.000015 ) M - matrix: 0.004639 0.000002 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000002 0.004626 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000012 -0.000003 0.004651 ( 0.000001 0.000001 0.000002 ) unit cell: 10.424(2) 10.438(2) 10.407(2) 89.885(17) 89.795(18) 90.205(17) V = 1132.4(4) unit cell: 10.4145(7) 10.4145(7) 10.4145(7) 90.0 90.0 90.0 V = 1129.57(14) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.938 ( 0.170) | 0.923 ( 0.398) | 1.01- 0.88 | 22 | 0.957 ( 0.073) | 1.004 ( 0.124) | 1.180 ( 0.493) | 0.88- 0.79 | 22 | 0.985 ( 0.059) | 1.028 ( 0.140) | 1.234 ( 0.387) | 0.79- 0.70 | 22 | 0.984 ( 0.041) | 0.962 ( 0.107) | 1.276 ( 0.475) | 0.70- 0.63 | 22 | 0.943 ( 0.038) | 0.917 ( 0.081) | 1.311 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 220 | 0.933 ( 0.193) | 0.943 ( 0.158) | 1.113 ( 0.914) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.86 | 25 | 0.946 ( 0.067) | 0.942 ( 0.097) | 1.046 ( 0.420) | 0.82- 0.73 | 25 | 0.957 ( 0.050) | 0.911 ( 0.086) | 1.356 ( 0.420) | 0.73- 0.63 | 28 | 0.929 ( 0.038) | 0.881 ( 0.096) | 1.353 ( 0.467) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 253 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.060 ( 0.485) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_6_51.rpb PROFFITPEAK info: 231 peaks in the peak location table UB fit with 83 obs out of 142 (total:142,skipped:0) (58.45%) UB - matrix: 0.066097 0.015164 0.006350 ( 0.000083 0.000127 0.000074 ) -0.016147 0.064484 0.013175 ( 0.000076 0.000118 0.000069 ) -0.003755 -0.014182 0.066507 ( 0.000088 0.000135 0.000079 ) M - matrix: 0.004644 0.000014 -0.000043 ( 0.000011 0.000010 0.000008 ) 0.000014 0.004589 0.000003 ( 0.000010 0.000016 0.000010 ) -0.000043 0.000003 0.004637 ( 0.000008 0.000010 0.000011 ) unit cell: 10.409(13) 10.470(17) 10.417(13) 90.04(12) 89.47(10) 90.18(12) V = 1135(3) UB fit with 83 obs out of 142 (total:142,skipped:0) (58.45%) UB - matrix: 0.066097 0.015164 0.006350 ( 0.000083 0.000127 0.000074 ) -0.016147 0.064484 0.013175 ( 0.000076 0.000118 0.000069 ) -0.003755 -0.014182 0.066507 ( 0.000088 0.000135 0.000079 ) M - matrix: 0.004644 0.000014 -0.000043 ( 0.000011 0.000010 0.000008 ) 0.000014 0.004589 0.000003 ( 0.000010 0.000016 0.000010 ) -0.000043 0.000003 0.004637 ( 0.000008 0.000010 0.000011 ) unit cell: 10.409(13) 10.470(17) 10.417(13) 90.04(12) 89.47(10) 90.18(12) V = 1135(3) OTKP changes: 56 1 1 1 OTKP changes: 56 1 1 1 OTKP changes: 56 1 1 1 No constraint UB - matrix: 0.065852 0.015643 0.006230 ( 0.000045 0.000048 0.000041 ) -0.016469 0.064474 0.012934 ( 0.000043 0.000046 0.000039 ) -0.002908 -0.014188 0.066469 ( 0.000026 0.000027 0.000024 ) M - matrix: 0.004616 0.000010 0.000004 ( 0.000006 0.000004 0.000003 ) 0.000010 0.004603 -0.000012 ( 0.000004 0.000006 0.000003 ) 0.000004 -0.000012 0.004624 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.065852 0.015643 0.006230 ( 0.000045 0.000048 0.000041 ) -0.016469 0.064474 0.012934 ( 0.000043 0.000046 0.000039 ) -0.002908 -0.014188 0.066469 ( 0.000026 0.000027 0.000024 ) M - matrix: 0.004619 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004619 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004619 ( 0.000000 0.000000 0.000002 ) UB fit with 132 obs out of 142 (total:142,skipped:0) (92.96%) unit cell: 10.440(7) 10.455(7) 10.431(4) 89.85(4) 90.05(4) 90.12(5) V = 1138(1) unit cell: 10.4417(19) 10.4417(19) 10.4417(19) 90.0 90.0 90.0 V = 1138.4(4) UB fit with 132 obs out of 142 (total:142,skipped:0) (92.96%) UB - matrix: 0.065852 0.015643 0.006230 ( 0.000045 0.000048 0.000041 ) -0.016469 0.064474 0.012934 ( 0.000043 0.000046 0.000039 ) -0.002908 -0.014188 0.066469 ( 0.000026 0.000027 0.000024 ) M - matrix: 0.004616 0.000010 0.000004 ( 0.000006 0.000004 0.000003 ) 0.000010 0.004603 -0.000012 ( 0.000004 0.000006 0.000003 ) 0.000004 -0.000012 0.004624 ( 0.000003 0.000003 0.000003 ) unit cell: 10.440(7) 10.455(7) 10.431(4) 89.85(4) 90.05(4) 90.12(5) V = 1138(1) OTKP changes: 61 1 1 1 OTKP changes: 61 1 1 1 No constraint UB - matrix: 0.065991 0.015609 0.006259 ( 0.000045 0.000047 0.000041 ) -0.016447 0.064595 0.012937 ( 0.000043 0.000046 0.000039 ) -0.002897 -0.014256 0.066583 ( 0.000030 0.000032 0.000027 ) M - matrix: 0.004634 0.000009 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000009 0.004619 -0.000016 ( 0.000004 0.000006 0.000003 ) 0.000007 -0.000016 0.004640 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: 0.065991 0.015609 0.006259 ( 0.000045 0.000047 0.000041 ) -0.016447 0.064595 0.012937 ( 0.000043 0.000046 0.000039 ) -0.002897 -0.014256 0.066583 ( 0.000030 0.000032 0.000027 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000002 ) UB fit with 132 obs out of 142 (total:142,skipped:0) (92.96%) unit cell: 10.420(7) 10.436(7) 10.413(4) 89.80(4) 90.09(4) 90.11(5) V = 1132(1) unit cell: 10.4231(19) 10.4231(19) 10.4231(19) 90.0 90.0 90.0 V = 1132.4(4) 142 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Run 6 Omega scan: (-99.000 - -24.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.032) HKL list info: 1026 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065991 0.015609 0.006259 ( 0.000045 0.000047 0.000041 ) -0.016447 0.064595 0.012937 ( 0.000043 0.000046 0.000039 ) -0.002897 -0.014256 0.066583 ( 0.000030 0.000032 0.000027 ) M - matrix: 0.004634 0.000009 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000009 0.004619 -0.000016 ( 0.000004 0.000006 0.000003 ) 0.000007 -0.000016 0.004640 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: 0.065991 0.015609 0.006259 ( 0.000045 0.000047 0.000041 ) -0.016447 0.064595 0.012937 ( 0.000043 0.000046 0.000039 ) -0.002897 -0.014256 0.066583 ( 0.000030 0.000032 0.000027 ) M - matrix: 0.004634 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004634 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004634 ( 0.000000 0.000000 0.000002 ) UB fit with 132 obs out of 142 (total:142,skipped:0) (92.96%) unit cell: 10.420(7) 10.436(7) 10.413(4) 89.80(4) 90.09(4) 90.11(5) V = 1132(1) unit cell: 10.4231(19) 10.4231(19) 10.4231(19) 90.0 90.0 90.0 V = 1132.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 132 obs out of 142 (total:142,skipped:0) (92.96%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_51.rpb 0 of 137 peaks identified as outliers and rejected 137 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 137 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 137 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 3.00 | 14 | 0.846 ( 0.125) | 0.854 ( 0.177) | 1.040 ( 0.477) | 2.58- 1.82 | 14 | 0.818 ( 0.109) | 0.845 ( 0.193) | 0.689 ( 0.291) | 1.76- 1.58 | 14 | 0.843 ( 0.105) | 0.854 ( 0.151) | 0.706 ( 0.257) | 1.58- 1.36 | 14 | 0.957 ( 0.092) | 0.993 ( 0.129) | 0.913 ( 0.245) | 1.36- 1.17 | 14 | 0.966 ( 0.104) | 1.007 ( 0.154) | 0.785 ( 0.238) | 1.16- 1.00 | 14 | 1.002 ( 0.073) | 1.030 ( 0.131) | 1.187 ( 0.425) | 1.00- 0.87 | 14 | 0.999 ( 0.085) | 0.997 ( 0.123) | 0.992 ( 0.332) | 0.87- 0.73 | 14 | 1.037 ( 0.036) | 1.051 ( 0.113) | 1.014 ( 0.399) | 0.73- 0.68 | 14 | 1.006 ( 0.054) | 0.897 ( 0.060) | 1.366 ( 0.561) | 0.68- 0.63 | 11 | 0.954 ( 0.049) | 0.859 ( 0.047) | 1.121 ( 0.367) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 137 | 0.943 ( 0.116) | 0.940 ( 0.158) | 0.978 ( 0.427) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 137 obs out of 137 (total:137,skipped:0) (100.00%) UB - matrix: 0.065951 0.015580 0.006293 ( 0.000026 0.000027 0.000025 ) -0.016390 0.064664 0.013034 ( 0.000028 0.000029 0.000027 ) -0.002827 -0.014145 0.066533 ( 0.000028 0.000029 0.000027 ) M - matrix: 0.004626 0.000008 0.000013 ( 0.000004 0.000003 0.000003 ) 0.000008 0.004624 -0.000000 ( 0.000003 0.000004 0.000003 ) 0.000013 -0.000000 0.004636 ( 0.000003 0.000003 0.000004 ) unit cell: 10.428(4) 10.431(4) 10.417(4) 90.00(3) 90.16(3) 90.09(3) V = 1133.1(8) OTKP changes: 137 1 1 1 OTKP changes: 137 1 1 1 No constraint UB - matrix: 0.066082 0.015577 0.006338 ( 0.000023 0.000023 0.000022 ) -0.016414 0.064716 0.012965 ( 0.000026 0.000026 0.000025 ) -0.002940 -0.014302 0.066664 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004645 0.000009 0.000010 ( 0.000003 0.000002 0.000002 ) 0.000009 0.004635 -0.000016 ( 0.000002 0.000004 0.000002 ) 0.000010 -0.000016 0.004652 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066082 0.015577 0.006338 ( 0.000023 0.000023 0.000022 ) -0.016414 0.064716 0.012965 ( 0.000026 0.000026 0.000025 ) -0.002940 -0.014302 0.066664 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000001 ) UB fit with 137 obs out of 137 (total:137,skipped:0) (100.00%) unit cell: 10.407(3) 10.418(4) 10.399(2) 89.81(2) 90.12(2) 90.11(3) V = 1127.5(6) unit cell: 10.4082(7) 10.4082(7) 10.4082(7) 90.0 90.0 90.0 V = 1127.54(14) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - -24.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=52.987) HKL list info: 1024 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066082 0.015577 0.006338 ( 0.000023 0.000023 0.000022 ) -0.016414 0.064716 0.012965 ( 0.000026 0.000026 0.000025 ) -0.002940 -0.014302 0.066664 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004645 0.000009 0.000010 ( 0.000003 0.000002 0.000002 ) 0.000009 0.004635 -0.000016 ( 0.000002 0.000004 0.000002 ) 0.000010 -0.000016 0.004652 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066082 0.015577 0.006338 ( 0.000023 0.000023 0.000022 ) -0.016414 0.064716 0.012965 ( 0.000026 0.000026 0.000025 ) -0.002940 -0.014302 0.066664 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000001 ) UB fit with 137 obs out of 137 (total:137,skipped:0) (100.00%) unit cell: 10.407(3) 10.418(4) 10.399(2) 89.81(2) 90.12(2) 90.11(3) V = 1127.5(6) unit cell: 10.4082(7) 10.4082(7) 10.4082(7) 90.0 90.0 90.0 V = 1127.54(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 137 obs out of 137 (total:137,skipped:0) (100.00%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_51.rpb 0 of 138 peaks identified as outliers and rejected 138 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 138 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 138 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.99 | 14 | 0.845 ( 0.124) | 0.853 ( 0.176) | 0.971 ( 0.515) | 2.58- 1.83 | 14 | 0.820 ( 0.115) | 0.842 ( 0.196) | 0.697 ( 0.291) | 1.76- 1.58 | 14 | 0.853 ( 0.105) | 0.857 ( 0.151) | 0.751 ( 0.235) | 1.58- 1.35 | 14 | 0.939 ( 0.096) | 0.960 ( 0.162) | 0.905 ( 0.261) | 1.35- 1.16 | 14 | 0.972 ( 0.085) | 0.991 ( 0.168) | 0.778 ( 0.228) | 1.16- 1.00 | 14 | 0.994 ( 0.075) | 1.015 ( 0.124) | 1.181 ( 0.374) | 1.00- 0.87 | 14 | 1.035 ( 0.070) | 1.044 ( 0.134) | 0.962 ( 0.294) | 0.87- 0.75 | 14 | 1.034 ( 0.036) | 1.023 ( 0.099) | 1.096 ( 0.477) | 0.73- 0.69 | 14 | 1.003 ( 0.051) | 0.910 ( 0.077) | 1.242 ( 0.535) | 0.68- 0.63 | 12 | 0.961 ( 0.054) | 0.861 ( 0.045) | 1.188 ( 0.390) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 138 | 0.945 ( 0.115) | 0.937 ( 0.160) | 0.974 ( 0.419) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.1 | 134 | 0.991 ( 0.040) | 1.036 ( 0.067) | 1.105 ( 0.463) | 10.2-14.8 | 134 | 0.994 ( 0.047) | 1.050 ( 0.070) | 1.111 ( 0.533) | 14.8-19.0 | 134 | 0.997 ( 0.184) | 1.037 ( 0.100) | 1.122 ( 0.971) | 19.0-23.4 | 134 | 0.972 ( 0.065) | 1.017 ( 0.086) | 0.933 ( 0.424) | 23.4-27.3 | 134 | 0.968 ( 0.067) | 0.998 ( 0.096) | 0.996 ( 0.460) | 27.3-32.2 | 134 | 0.942 ( 0.084) | 0.958 ( 0.105) | 0.941 ( 0.443) | 32.2-36.3 | 134 | 0.927 ( 0.154) | 0.917 ( 0.145) | 1.078 ( 0.663) | 36.3-38.9 | 134 | 0.886 ( 0.106) | 0.879 ( 0.250) | 1.007 ( 0.481) | 38.9-41.9 | 134 | 0.899 ( 0.098) | 0.843 ( 0.130) | 1.002 ( 0.439) | 41.9-50.1 | 137 | 0.867 ( 0.123) | 0.796 ( 0.141) | 0.934 ( 0.442) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1343 | 0.944 ( 0.116) | 0.953 ( 0.155) | 1.023 ( 0.560) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.14 e2 dimension: a=-0.0070 b=1.24 e3 dimension: a=0.0006 b=1.10 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 4496 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 14:38:15 2019 PROFFITMAIN - Started at Wed Aug 21 14:38:15 2019 OTKP changes: 1033 2 5 6 OTKP changes: 1033 2 5 6 OTKP changes: 1033 2 5 6 No constraint UB - matrix: 0.066124 0.015050 0.006706 ( 0.000013 0.000015 0.000014 ) -0.016124 0.064810 0.013164 ( 0.000013 0.000014 0.000013 ) -0.003731 -0.014364 0.066607 ( 0.000015 0.000016 0.000015 ) M - matrix: 0.004646 0.000004 -0.000017 ( 0.000002 0.000001 0.000001 ) 0.000004 0.004633 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000017 -0.000003 0.004655 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066124 0.015050 0.006706 ( 0.000013 0.000015 0.000014 ) -0.016124 0.064810 0.013164 ( 0.000013 0.000014 0.000013 ) -0.003731 -0.014364 0.066607 ( 0.000015 0.000016 0.000015 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 1062 obs out of 1343 (total:1343,skipped:0) (79.08%) unit cell: 10.406(2) 10.421(2) 10.396(2) 89.968(17) 89.787(17) 90.047(16) V = 1127.3(4) unit cell: 10.4076(7) 10.4076(7) 10.4076(7) 90.0 90.0 90.0 V = 1127.34(14) *** 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 187 obs out of 220 (total:220,skipped:0) (85.00%) UB - matrix: 0.066500 0.011702 0.008960 ( 0.000032 0.000043 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000030 0.000040 0.000034 ) -0.006052 -0.013931 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.60(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004603 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 220 (total:220,skipped:0) (85.91%) unit cell: 10.406(5) 10.502(6) 10.456(6) 90.61(5) 90.19(4) 89.64(4) V = 1143(1) unit cell: 10.4543(19) 10.4543(19) 10.4543(19) 90.0 90.0 90.0 V = 1142.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 220 (total:220,skipped:0) (92.27%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004644 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 220 (total:220,skipped:0) (93.64%) unit cell: 10.409(4) 10.492(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1140.0(9) unit cell: 10.4466(13) 10.4466(13) 10.4466(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.066336 0.014185 0.006781 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064703 0.012861 ( 0.000017 0.000023 0.000023 ) -0.004076 -0.014198 0.066902 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 No constraint UB - matrix: 0.066343 0.014186 0.006784 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014200 0.066900 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066343 0.014186 0.006784 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014200 0.066900 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.11(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066343 0.014186 0.006784 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014200 0.066900 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066343 0.014186 0.006784 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014200 0.066900 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.11(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068244 -0.000102 -0.000276 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000012 0.000000 0.068378 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068244 -0.000102 -0.000276 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000012 0.000000 0.068378 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.394(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4048(5) 10.4048(5) 10.4048(5) 90.0 90.0 90.0 V = 1126.41(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065876 0.015198 0.006804 ( 0.000019 0.000013 0.000019 ) -0.016068 0.064775 0.013238 ( 0.000017 0.000012 0.000016 ) -0.003643 -0.014502 0.066492 ( 0.000021 0.000015 0.000020 ) M - matrix: 0.004611 0.000013 -0.000007 ( 0.000003 0.000001 0.000002 ) 0.000013 0.004637 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000007 -0.000003 0.004643 ( 0.000002 0.000001 0.000003 ) unit cell: 10.446(3) 10.416(2) 10.410(3) 89.959(19) 89.92(2) 90.163(18) V = 1132.6(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065912 0.015211 0.006788 ( 0.000019 0.000013 0.000019 ) -0.016108 0.064823 0.013253 ( 0.000016 0.000011 0.000016 ) -0.003644 -0.014464 0.066548 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004617 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004643 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004650 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065912 0.015211 0.006788 ( 0.000019 0.000013 0.000019 ) -0.016108 0.064823 0.013253 ( 0.000016 0.000011 0.000016 ) -0.003644 -0.014464 0.066548 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004641 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004641 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004641 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.439(3) 10.4100(19) 10.401(3) 89.998(18) 89.89(2) 90.137(18) V = 1130.3(5) unit cell: 10.4166(5) 10.4166(5) 10.4166(5) 90.0 90.0 90.0 V = 1130.27(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.063) HKL list info: 1275 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065912 0.015211 0.006788 ( 0.000019 0.000013 0.000019 ) -0.016108 0.064823 0.013253 ( 0.000016 0.000011 0.000016 ) -0.003644 -0.014464 0.066548 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004617 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004643 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004650 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065912 0.015211 0.006788 ( 0.000019 0.000013 0.000019 ) -0.016108 0.064823 0.013253 ( 0.000016 0.000011 0.000016 ) -0.003644 -0.014464 0.066548 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004641 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004641 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004641 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.439(3) 10.4100(19) 10.401(3) 89.998(18) 89.89(2) 90.137(18) V = 1130.3(5) unit cell: 10.4166(5) 10.4166(5) 10.4166(5) 90.0 90.0 90.0 V = 1130.27(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065912 0.015211 0.006788 ( 0.000019 0.000013 0.000019 ) -0.016108 0.064823 0.013253 ( 0.000016 0.000011 0.000016 ) -0.003644 -0.014464 0.066548 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004617 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004643 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004650 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065912 0.015211 0.006788 ( 0.000019 0.000013 0.000019 ) -0.016108 0.064823 0.013253 ( 0.000016 0.000011 0.000016 ) -0.003644 -0.014464 0.066548 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004641 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004641 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004641 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.439(3) 10.4100(19) 10.401(3) 89.998(18) 89.89(2) 90.137(18) V = 1130.3(5) unit cell: 10.4166(5) 10.4166(5) 10.4166(5) 90.0 90.0 90.0 V = 1130.27(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066108 0.015244 0.006579 ( 0.000015 0.000020 0.000017 ) -0.016342 0.064730 0.012930 ( 0.000012 0.000016 0.000013 ) -0.003358 -0.014197 0.066510 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004649 -0.000002 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000002 0.004624 -0.000007 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000007 0.004634 ( 0.000001 0.000001 0.000002 ) unit cell: 10.403(2) 10.431(2) 10.4196(18) 89.914(16) 90.003(17) 89.971(19) V = 1130.7(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066130 0.015254 0.006531 ( 0.000013 0.000018 0.000015 ) -0.016355 0.064766 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003350 -0.014170 0.066585 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004652 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004628 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004644 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066130 0.015254 0.006531 ( 0.000013 0.000018 0.000015 ) -0.016355 0.064766 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003350 -0.014170 0.066585 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.400(2) 10.426(2) 10.4082(18) 89.946(16) 89.961(15) 89.963(18) V = 1128.5(4) unit cell: 10.4113(5) 10.4113(5) 10.4113(5) 90.0 90.0 90.0 V = 1128.55(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.063) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066130 0.015254 0.006531 ( 0.000013 0.000018 0.000015 ) -0.016355 0.064766 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003350 -0.014170 0.066585 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004652 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004628 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004644 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066130 0.015254 0.006531 ( 0.000013 0.000018 0.000015 ) -0.016355 0.064766 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003350 -0.014170 0.066585 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.400(2) 10.426(2) 10.4082(18) 89.946(16) 89.961(15) 89.963(18) V = 1128.5(4) unit cell: 10.4113(5) 10.4113(5) 10.4113(5) 90.0 90.0 90.0 V = 1128.55(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068190 -0.000040 -0.000036 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068045 -0.000052 ( 0.000013 0.000018 0.000015 ) 0.000008 0.000010 0.068150 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004650 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004630 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004644 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068190 -0.000040 -0.000036 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068045 -0.000052 ( 0.000013 0.000018 0.000015 ) 0.000008 0.000010 0.068150 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.4019(16) 10.424(3) 10.4080(15) 89.964(16) 89.976(13) 89.967(17) V = 1128.5(4) unit cell: 10.4113(5) 10.4113(5) 10.4113(5) 90.0 90.0 90.0 V = 1128.52(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 249 obs out of 271 (total:271,skipped:0) (91.88%) UB - matrix: 0.065948 0.015324 0.006330 ( 0.000017 0.000013 0.000013 ) -0.016399 0.064810 0.013396 ( 0.000021 0.000016 0.000016 ) -0.003138 -0.014517 0.066485 ( 0.000029 0.000022 0.000022 ) M - matrix: 0.004628 -0.000007 -0.000011 ( 0.000002 0.000002 0.000002 ) -0.000007 0.004646 0.000000 ( 0.000002 0.000002 0.000002 ) -0.000011 0.000000 0.004640 ( 0.000002 0.000002 0.000003 ) unit cell: 10.426(3) 10.406(3) 10.413(3) 90.00(2) 89.87(3) 89.92(2) V = 1129.8(5) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.066025 0.015376 0.006324 ( 0.000016 0.000012 0.000013 ) -0.016382 0.064822 0.013382 ( 0.000018 0.000013 0.000014 ) -0.002870 -0.014636 0.066537 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004636 -0.000005 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004653 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004646 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066025 0.015376 0.006324 ( 0.000016 0.000012 0.000013 ) -0.016382 0.064822 0.013382 ( 0.000018 0.000013 0.000014 ) -0.002870 -0.014636 0.066537 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.417(2) 10.399(2) 10.4059(18) 89.887(15) 90.091(17) 89.942(18) V = 1127.3(4) unit cell: 10.4074(5) 10.4074(5) 10.4074(5) 90.0 90.0 90.0 V = 1127.26(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.063) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066025 0.015376 0.006324 ( 0.000016 0.000012 0.000013 ) -0.016382 0.064822 0.013382 ( 0.000018 0.000013 0.000014 ) -0.002870 -0.014636 0.066537 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004636 -0.000005 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004653 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004646 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066025 0.015376 0.006324 ( 0.000016 0.000012 0.000013 ) -0.016382 0.064822 0.013382 ( 0.000018 0.000013 0.000014 ) -0.002870 -0.014636 0.066537 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.417(2) 10.399(2) 10.4059(18) 89.887(15) 90.091(17) 89.942(18) V = 1127.3(4) unit cell: 10.4074(5) 10.4074(5) 10.4074(5) 90.0 90.0 90.0 V = 1127.26(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068095 -0.000092 0.000069 ( 0.000017 0.000013 0.000014 ) 0.000058 0.068179 -0.000091 ( 0.000014 0.000010 0.000011 ) -0.000018 0.000008 0.068156 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004637 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004648 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004645 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068095 -0.000092 0.000069 ( 0.000017 0.000013 0.000014 ) 0.000058 0.068179 -0.000091 ( 0.000014 0.000010 0.000011 ) -0.000018 0.000008 0.068156 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.416(3) 10.4035(16) 10.4071(18) 89.931(13) 90.044(17) 89.971(16) V = 1127.8(4) unit cell: 10.4090(5) 10.4090(5) 10.4090(5) 90.0 90.0 90.0 V = 1127.78(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 138 obs out of 138 (total:138,skipped:0) (100.00%) UB - matrix: 0.066082 0.015575 0.006333 ( 0.000024 0.000024 0.000023 ) -0.016411 0.064714 0.012966 ( 0.000026 0.000027 0.000025 ) -0.002941 -0.014296 0.066662 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004645 0.000009 0.000010 ( 0.000003 0.000002 0.000002 ) 0.000009 0.004635 -0.000015 ( 0.000002 0.000004 0.000002 ) 0.000010 -0.000015 0.004652 ( 0.000002 0.000002 0.000002 ) unit cell: 10.408(4) 10.419(4) 10.399(2) 89.81(2) 90.12(2) 90.11(3) V = 1127.6(6) OTKP changes: 138 1 1 1 OTKP changes: 138 1 1 1 No constraint UB - matrix: 0.066104 0.015572 0.006337 ( 0.000024 0.000024 0.000023 ) -0.016410 0.064733 0.012964 ( 0.000026 0.000027 0.000025 ) -0.002947 -0.014305 0.066678 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004648 0.000009 0.000010 ( 0.000003 0.000002 0.000002 ) 0.000009 0.004637 -0.000016 ( 0.000002 0.000004 0.000002 ) 0.000010 -0.000016 0.004654 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066104 0.015572 0.006337 ( 0.000024 0.000024 0.000023 ) -0.016410 0.064733 0.012964 ( 0.000026 0.000027 0.000025 ) -0.002947 -0.014305 0.066678 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004651 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004651 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004651 ( 0.000000 0.000000 0.000001 ) UB fit with 138 obs out of 138 (total:138,skipped:0) (100.00%) unit cell: 10.404(4) 10.416(4) 10.397(2) 89.80(2) 90.12(2) 90.11(3) V = 1126.7(6) unit cell: 10.4057(7) 10.4057(7) 10.4057(7) 90.0 90.0 90.0 V = 1126.73(13) Run 6 Omega scan: (-99.000 - -24.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=52.972) HKL list info: 1002 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066104 0.015572 0.006337 ( 0.000024 0.000024 0.000023 ) -0.016410 0.064733 0.012964 ( 0.000026 0.000027 0.000025 ) -0.002947 -0.014305 0.066678 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004648 0.000009 0.000010 ( 0.000003 0.000002 0.000002 ) 0.000009 0.004637 -0.000016 ( 0.000002 0.000004 0.000002 ) 0.000010 -0.000016 0.004654 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066104 0.015572 0.006337 ( 0.000024 0.000024 0.000023 ) -0.016410 0.064733 0.012964 ( 0.000026 0.000027 0.000025 ) -0.002947 -0.014305 0.066678 ( 0.000016 0.000016 0.000015 ) M - matrix: 0.004651 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004651 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004651 ( 0.000000 0.000000 0.000001 ) UB fit with 138 obs out of 138 (total:138,skipped:0) (100.00%) unit cell: 10.404(4) 10.416(4) 10.397(2) 89.80(2) 90.12(2) 90.11(3) V = 1126.7(6) unit cell: 10.4057(7) 10.4057(7) 10.4057(7) 90.0 90.0 90.0 V = 1126.73(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 138 obs out of 138 (total:138,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: 0.068188 0.000113 0.000139 ( 0.000024 0.000025 0.000024 ) -0.000018 0.068116 -0.000223 ( 0.000024 0.000025 0.000023 ) 0.000001 -0.000005 0.068218 ( 0.000014 0.000014 0.000013 ) M - matrix: 0.004650 0.000006 0.000010 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004640 -0.000015 ( 0.000002 0.000003 0.000002 ) 0.000010 -0.000015 0.004654 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.068188 0.000113 0.000139 ( 0.000024 0.000025 0.000024 ) -0.000018 0.068116 -0.000223 ( 0.000024 0.000025 0.000023 ) 0.000001 -0.000005 0.068218 ( 0.000014 0.000014 0.000013 ) M - matrix: 0.004651 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004651 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004651 ( 0.000000 0.000000 0.000001 ) UB fit with 138 obs out of 138 (total:138,skipped:0) (100.00%) unit cell: 10.402(4) 10.413(4) 10.398(2) 89.81(2) 90.12(2) 90.08(3) V = 1126.3(6) unit cell: 10.4043(7) 10.4043(7) 10.4043(7) 90.0 90.0 90.0 V = 1126.25(13) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_51.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068156 0.000022 -0.000058 ( 0.000009 0.000009 0.000009 ) -0.000001 0.068076 0.000001 ( 0.000010 0.000010 0.000010 ) 0.000028 -0.000020 0.068163 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004645 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.004634 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000001 0.004646 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068156 0.000022 -0.000058 ( 0.000009 0.000009 0.000009 ) -0.000001 0.068076 0.000001 ( 0.000010 0.000010 0.000010 ) 0.000028 -0.000020 0.068163 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) UB fit with 1319 obs out of 1343 (total:1343,skipped:0) (98.21%) unit cell: 10.4071(13) 10.4193(16) 10.4059(11) 89.984(10) 89.975(10) 90.017(11) V = 1128.4(2) unit cell: 10.4108(3) 10.4108(3) 10.4108(3) 90.0 90.0 90.0 V = 1128.36(6) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 144 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof 5911 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:38:25 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.063) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.063) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.063) Run 6 Omega scan: (-99.000 - -24.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=52.972) PROFFIT INFO: signal sum: min=-775.0000 max=7910405.0000 PROFFIT INFO: signal sum lp corr: min=-663.2892 max=1261985.2081 PROFFIT INFO: background sum: min=-84.0000 max=8197.0000 PROFFIT INFO: background sum sig2: min=414.0000 max=5795.0000 PROFFIT INFO: num of signal pixels: min=41 max=519 PROFFIT INFO: Inet: min=-1061.2627 max=2019176.3750 PROFFIT INFO: sig(Inet): min=51.9729 max=30716.7539 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=277.22 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 505 2031 3072 3664 3950 4586 4985 5232 5601 5847 5911 Percent 8.5 34.4 52.0 62.0 66.8 77.6 84.3 88.5 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5911 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 5911 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2019176- 129129 591 413512.15 77.68 100.00 128887- 4056 591 28927.03 19.51 100.00 4050- 2039 591 2867.90 7.08 96.79 2033- 1236 591 1582.88 3.93 53.13 1235- 813 591 1004.55 2.34 15.74 813- 540 591 671.22 1.75 8.63 539- 338 591 433.00 1.21 4.91 338- 154 591 245.51 0.72 1.02 154- 21 591 82.57 0.30 0.00 21- -1061 592 -131.52 -0.25 0.00 ------------------------------------------------------------------------------------ 2019176- -1061 5911 44911.91 11.42 38.01 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 591 113184.61 15.84 68.70 1.73- 1.26 591 86240.17 21.53 59.56 1.26- 1.09 591 59660.98 18.30 66.67 1.09- 0.96 591 55013.36 14.96 34.69 0.96- 0.88 591 17116.29 6.97 44.16 0.88- 0.80 591 50064.54 14.15 36.38 0.80- 0.76 591 18727.16 5.84 18.95 0.76- 0.71 591 20996.14 6.82 16.24 0.71- 0.67 591 24582.79 8.04 28.60 0.67- 0.63 592 3602.92 1.78 6.25 ------------------------------------------------------------------------------------ 6.00- 0.63 5911 44911.91 11.42 38.01 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:38:25 2019 Sorting 5911 observations 53 unique observations with > 7.00 F2/sig(F2) 5911 observations in 6 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 74 590 Total number of frames 590 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 12 frame = 1 scale 5911 observations in 6 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 6 0 6 52 Total number of frames 52 1425 observations > 7.00 F2/sig(F2) 1425 observations in 6 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 6 0 6 52 Total number of frames 52 Removing 'redundancy=1' reflections Average redundancy: 21.1 (Out of 1425 removed 8 = 1417, unique = 67) 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 1417 observations in 6 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 6 0 6 52 Total number of frames 52 67 unique data precomputed (should be 67) 67 unique data with 1417 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 21.1 (Out of 1417 removed 0 = 1417, unique = 67) 67 unique data precomputed (should be 67) 67 unique data with 1417 observations RMS deviation of equivalent data = 0.31285 Rint = 0.26042 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.25120, wR= 0.34531 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13379, wR= 0.18939, Acormin=0.463, Acormax=1.412, Acor_av=1.002 F test: Probability=1.000, F= 3.512 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12243, wR= 0.17618, Acormin=0.441, Acormax=1.472, Acor_av=0.963 F test: Probability=0.999, F= 1.191 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12574, wR= 0.17907, Acormin=0.534, Acormax=1.530, Acor_av=0.997 F test: Probability=0.000, F= 0.944 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10887, wR= 0.16152, Acormin=0.411, Acormax=1.593, Acor_av=0.964 F test: Probability=1.000, F= 1.256 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09512, wR= 0.14727, Acormin=0.521, Acormax=1.810, Acor_av=1.006 F test: Probability=1.000, F= 1.303 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11736, wR= 0.16966, Acormin=0.401, Acormax=1.599, Acor_av=0.970 F test: Probability=0.000, F= 0.655 Trying model 7 (ne=6, no=1)... Results: Rint= 0.10507, wR= 0.15555, Acormin=0.391, Acormax=1.653, Acor_av=0.952 F test: Probability=0.000, F= 0.816 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09116, wR= 0.14266, Acormin=0.464, Acormax=1.792, Acor_av=0.990 F test: Probability=0.913, F= 1.078 Trying model 9 (ne=6, no=5)... Results: Rint= 0.15502, wR= 0.19399, Acormin=0.011, Acormax=1.061, Acor_av=0.470 F test: Probability=0.000, F= 0.370 Final absorption model (ne=4, no=3): Rint= 0.09512, Acormin=0.521, Acormax=1.810, Acor_av=1.006 Combined refinement in use Rint: 0.26216 There are 52 active scales (one needs to be fixed) Refinement control: frame scale #41 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 75 pars with 2850 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31285 Using Levenberg-Marquardt: 0.00010 New wR= 0.10860 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.26042 with corrections 0.07864 Rint for all data: 0.26216 with corrections 0.08136 3 observations identified as outliers and rejected Cycle 2 wR= 0.09891 Using Levenberg-Marquardt: 0.00001 New wR= 0.08303 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.26027 with corrections 0.05636 Rint for all data: 0.26216 with corrections 0.06210 2 observations identified as outliers and rejected Cycle 3 wR= 0.07640 Using Levenberg-Marquardt: 0.00000 New wR= 0.07377 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25948 with corrections 0.05143 Rint for all data: 0.26216 with corrections 0.05770 2 observations identified as outliers and rejected Cycle 4 wR= 0.06743 Using Levenberg-Marquardt: 0.00000 New wR= 0.06585 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25787 with corrections 0.04566 Rint for all data: 0.26216 with corrections 0.05307 1 observations identified as outliers and rejected Cycle 5 wR= 0.06260 Using Levenberg-Marquardt: 0.00000 New wR= 0.06128 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25737 with corrections 0.04353 Rint for all data: 0.26216 with corrections 0.05137 0 observations identified as outliers and rejected Final wR= 0.06128 Final frame scales: Min= 0.6609 Max= 1.3852 Final absorption correction factors: Amin= 0.3889 Amax= 1.6045 PROFFIT INFO: Inet (after scale3 abspack): min=-1084.1284 max=1232901.8750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=37.7522 max=24148.4102 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/104 5911 reflections read from tmp file 205 reflections are rejected (204 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 3 5 4 4 5 2 3 211 Initial Chi^2= 0.51632 Cycle 1, Chi^2= 1.03619 Current error model SIG(F2)^2 = 64.05*I_RAW + 10.48*I_BACK+(0.02649*)^2 Cycle 2, Chi^2= 1.01884 Current error model SIG(F2)^2 = 77.78*I_RAW + 7.12*I_BACK+(0.02360*)^2 Cycle 3, Chi^2= 1.00634 Current error model SIG(F2)^2 = 82.29*I_RAW + 6.29*I_BACK+(0.02309*)^2 Cycle 4, Chi^2= 1.00186 Current error model SIG(F2)^2 = 83.63*I_RAW + 6.06*I_BACK+(0.02301*)^2 Cycle 5, Chi^2= 1.00054 Current error model SIG(F2)^2 = 84.01*I_RAW + 6.00*I_BACK+(0.02298*)^2 Cycle 6, Chi^2= 1.00016 Current error model SIG(F2)^2 = 84.12*I_RAW + 5.98*I_BACK+(0.02298*)^2 Final Chi^2= 1.00016 Final error model SIG(F2)^2 = 84.12*I_RAW + 5.98*I_BACK+(0.02298*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1232902- 115700 591 376021.51 33.65 100.00 115091- 3407 591 28605.54 13.44 100.00 3407- 2006 591 2641.99 6.27 99.49 2002- 1146 591 1496.83 3.98 66.33 1146- 767 591 937.15 2.81 28.09 766- 513 591 635.76 2.42 17.26 513- 324 591 414.01 1.97 9.31 324- 149 591 238.51 1.47 3.05 149- 21 591 80.92 0.75 0.51 21- -1084 592 -131.66 -0.54 0.00 ------------------------------------------------------------------------------------ 1232902- -1084 5911 41087.08 6.62 42.40 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 591 104613.41 10.89 71.91 1.73- 1.26 591 78827.65 10.17 63.45 1.26- 1.09 591 54919.34 8.72 71.74 1.09- 0.96 591 49680.08 7.16 37.06 0.96- 0.88 591 15384.49 4.94 52.62 0.88- 0.80 591 46094.95 7.96 43.32 0.80- 0.76 591 17224.88 4.05 22.34 0.76- 0.71 591 18691.25 4.97 20.98 0.71- 0.67 591 22181.54 5.62 32.66 0.67- 0.63 592 3317.14 1.74 7.94 ------------------------------------------------------------------------------------ 6.00- 0.63 5911 41087.08 6.62 42.40 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 591 104613.41 10.89 71.91 6.00- 1.26 1182 91720.53 10.53 67.68 6.00- 1.09 1773 79453.47 9.92 69.04 6.00- 0.96 2364 72010.12 9.23 61.04 6.00- 0.88 2955 60684.99 8.37 59.36 6.00- 0.80 3546 58253.32 8.30 56.68 6.00- 0.76 4137 52392.11 7.70 51.78 6.00- 0.71 4728 48179.51 7.36 47.93 6.00- 0.67 5319 45290.84 7.16 46.23 6.00- 0.63 5911 41087.08 6.62 42.40 ------------------------------------------------------------------------------------ 6.00- 0.63 5911 41087.08 6.62 42.40 Scale applied to data: s=0.811094 (maximum obs:1232901.875,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.051; Rsigma 0.035: data 5911 -> merged 240 With outlier rejection... Rint 0.045; Rsigma 0.035: data 5889 -> merged 240 Rejected total: 22, method kkm 13, method Blessing 9 Completeness direct cell (a, b, c) = (10.411, 10.411, 10.411), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626654, 6.010649 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.41 - 1.59 21 21 32.43 100.00 681 1.57 - 1.20 21 21 33.52 100.00 704 1.19 - 1.02 21 21 31.52 100.00 662 1.02 - 0.91 21 21 30.00 100.00 630 0.91 - 0.84 21 21 26.62 100.00 559 0.84 - 0.78 21 21 26.24 100.00 551 0.78 - 0.74 21 21 24.90 100.00 523 0.74 - 0.71 21 21 20.90 100.00 439 0.71 - 0.68 21 21 23.10 100.00 485 0.68 - 0.65 23 23 19.61 100.00 451 --------------------------------------------------------------- 10.41 - 0.65 212 212 26.82 100.00 5685 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:38:25 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.407061 10.419285 10.405912 89.9842 89.9750 90.0170 5889 Reflections read from file xs2212a.hkl 5854 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.63 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2940 0 3882 3880 5854 N (int>3sigma) = 0 0 0 0 1331 0 1744 1728 2489 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 34.5 32.3 33.3 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.8 6.7 6.6 Lattice type: F chosen Volume: 1128.36 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.357 7.360 7.362 119.99 119.96 90.01 Niggli form: a.a = 54.124 b.b = 54.171 c.c = 54.196 b.c = -27.083 a.c = -27.043 a.b = -0.006 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.092 CUBIC F-lattice R(int) = 0.045 [ 5623] Vol = 1128.4 Cell: 10.419 10.407 10.406 89.97 90.02 89.98 Volume: 1128.36 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.091 TETRAGONAL I-lattice R(int) = 0.045 [ 5237] Vol = 564.2 Cell: 7.362 7.364 10.406 90.01 89.97 89.93 Volume: 564.18 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.055 TETRAGONAL I-lattice R(int) = 0.044 [ 5238] Vol = 564.2 Cell: 7.357 7.360 10.419 90.00 89.98 90.01 Volume: 564.18 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.075 TETRAGONAL I-lattice R(int) = 0.045 [ 5237] Vol = 564.2 Cell: 7.364 7.362 10.406 90.03 90.01 90.07 Volume: 564.18 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.061 ORTHORHOMBIC F-lattice R(int) = 0.044 [ 5184] Vol = 1128.4 Cell: 10.406 10.407 10.419 89.98 90.02 89.97 Volume: 1128.36 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.101 ORTHORHOMBIC I-lattice R(int) = 0.043 [ 5164] Vol = 564.2 Cell: 10.406 7.364 7.362 89.93 89.97 90.01 Volume: 564.18 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.020 ORTHORHOMBIC I-lattice R(int) = 0.043 [ 5166] Vol = 564.2 Cell: 7.357 7.360 10.419 90.00 90.02 90.01 Volume: 564.18 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.056 MONOCLINIC I-lattice R(int) = 0.042 [ 4639] Vol = 564.2 Cell: 7.362 10.406 7.364 90.01 90.07 90.03 Volume: 564.18 Matrix:-0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.056 MONOCLINIC I-lattice R(int) = 0.043 [ 4638] Vol = 564.2 Cell: 7.362 10.407 7.364 89.99 90.07 89.97 Volume: 564.18 Matrix: 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.049 MONOCLINIC I-lattice R(int) = 0.042 [ 4639] Vol = 564.2 Cell: 7.364 10.406 7.362 90.03 90.07 90.01 Volume: 564.18 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.006 MONOCLINIC I-lattice R(int) = 0.041 [ 4627] Vol = 564.2 Cell: 7.357 7.360 10.419 90.00 90.02 89.99 Volume: 564.18 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.016 MONOCLINIC I-lattice R(int) = 0.042 [ 4641] Vol = 564.2 Cell: 7.357 10.419 7.360 90.00 90.01 89.98 Volume: 564.18 Matrix: 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.039 MONOCLINIC I-lattice R(int) = 0.042 [ 4641] Vol = 564.2 Cell: 7.357 10.419 7.360 90.00 90.01 90.02 Volume: 564.18 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) = 0.037 [ 3583] Vol = 282.1 Cell: 7.357 7.360 7.362 119.99 119.96 90.01 Volume: 282.09 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -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 2940 0 3893 3899 5854 N (int>3sigma) = 0 0 0 0 1331 0 1765 1754 2489 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 32.8 34.3 33.3 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.7 6.8 6.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.424 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 39 39 423 1157 N I>3s 2 2 2 630 0.0 0.0 0.0 2.1 0.8 0.8 0.2 5.2 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 0.045 5228 Fd-3m 1 1 227 C N N N N 37 2284 0.045 5290 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.419285 10.407061 10.405912 89.9750 90.0158 89.9830 ZERR 5.00 0.001555 0.001328 0.001108 0.0096 0.0105 0.0112 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1133945- 127367 586 577 26 22.2 379410.85 33.83 0.040 0.050 106867- 3079 672 666 26 25.6 26412.65 12.62 0.064 0.075 2997- 1361 859 856 26 32.9 2181.12 5.66 0.124 0.178 1357- 855 736 736 26 28.3 1039.07 2.80 0.235 0.307 816- 486 746 745 26 28.7 636.37 2.38 0.297 0.401 486- 293 713 713 26 27.4 375.80 1.72 0.449 0.616 288- 155 498 498 26 19.2 226.41 1.34 0.572 0.936 144- 26 623 623 26 24.0 78.44 0.58 0.867 2.451 23- -165 478 475 32 14.8 -27.81 -0.06 0.999 4.148 ------------------------------------------------------------------------------------------- 1133945- -165 5911 5889 240 24.5 40759.57 6.59 0.045 0.056 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-1.44 872 869 26 33.4 115034.59 12.15 0.038 0.045 0.026 1.39-1.09 904 901 26 34.7 43377.76 7.67 0.041 0.050 0.032 1.06-0.94 757 754 26 29.0 38612.85 6.12 0.043 0.051 0.033 0.92-0.84 713 710 26 27.3 41232.63 7.88 0.047 0.060 0.039 0.84-0.78 696 694 26 26.7 23975.57 5.25 0.055 0.072 0.045 0.78-0.73 596 596 26 22.9 8374.38 3.17 0.076 0.093 0.074 0.73-0.69 621 620 27 23.0 18621.12 4.76 0.063 0.077 0.059 0.68-0.66 538 535 27 19.8 14690.00 4.04 0.080 0.113 0.065 0.65-0.63 214 210 30 7.0 7433.50 2.42 0.077 0.077 0.087 ------------------------------------------------------------------------------------------------------ inf-0.63 5911 5889 240 24.5 40759.57 6.59 0.045 0.056 0.035 inf-0.65 5701 5683 211 26.9 42026.22 6.76 0.045 0.056 0.034 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-1.44 869 26 26 100.0 33.4 115034.59 70.37 0.038 0.005 1.39-1.09 901 26 26 100.0 34.7 43377.76 40.74 0.041 0.007 1.06-0.94 754 26 26 100.0 29.0 38612.85 34.11 0.043 0.007 0.92-0.84 710 26 26 100.0 27.3 41232.63 40.91 0.047 0.008 0.84-0.78 694 26 26 100.0 26.7 23975.57 25.77 0.055 0.009 0.78-0.73 596 26 26 100.0 22.9 8374.38 15.21 0.076 0.016 0.73-0.69 620 27 27 100.0 23.0 18621.12 21.45 0.063 0.013 0.68-0.66 535 27 27 100.0 19.8 14690.00 19.63 0.080 0.015 0.65-0.63 210 30 30 100.0 7.0 7433.50 5.95 0.077 0.035 -------------------------------------------------------------------------------------------- inf-0.63 5889 240 240 100.0 24.5 40759.57 34.75 0.045 0.008 inf-0.65 5683 211 211 100.0 26.9 42026.22 35.82 0.045 0.008 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066121 0.015017 0.006880 ( 0.000009 0.000009 0.000009 ) -0.016111 0.064819 0.013171 ( 0.000010 0.000010 0.000010 ) -0.003675 -0.014403 0.066524 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004645 0.000002 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000002 0.004634 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000001 0.004646 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066121 0.015017 0.006880 ( 0.000009 0.000009 0.000009 ) -0.016111 0.064819 0.013171 ( 0.000010 0.000010 0.000010 ) -0.003675 -0.014403 0.066524 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4072(13) 10.4191(15) 10.4059(11) 89.986(10) 89.978(9) 90.019(11) V = 1128.4(2) unit cell: 10.4107(3) 10.4107(3) 10.4107(3) 90.0 90.0 90.0 V = 1128.35(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.063) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.063) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.063) Run 6 Omega scan: (-99.000 - -24.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=52.972) PROFFIT INFO: signal sum: min=-775.0000 max=7910405.0000 PROFFIT INFO: signal sum lp corr: min=-663.2892 max=1261985.2081 PROFFIT INFO: background sum: min=-84.0000 max=8197.0000 PROFFIT INFO: background sum sig2: min=414.0000 max=5795.0000 PROFFIT INFO: num of signal pixels: min=41 max=519 PROFFIT INFO: Inet: min=-1061.2627 max=2019176.3750 PROFFIT INFO: sig(Inet): min=51.9729 max=30716.7539 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=277.22 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 1010 4062 6144 7328 7900 9172 9970 10464 11202 11694 11822 Percent 8.5 34.4 52.0 62.0 66.8 77.6 84.3 88.5 94.8 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 5911 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 5911 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2019176- 129129 591 413512.15 77.68 100.00 128887- 4056 591 28927.03 19.51 100.00 4050- 2039 591 2867.90 7.08 96.79 2033- 1236 591 1582.88 3.93 53.13 1235- 813 591 1004.55 2.34 15.74 813- 540 591 671.22 1.75 8.63 539- 338 591 433.00 1.21 4.91 338- 154 591 245.51 0.72 1.02 154- 21 591 82.57 0.30 0.00 21- -1061 592 -131.52 -0.25 0.00 ------------------------------------------------------------------------------------ 2019176- -1061 5911 44911.91 11.42 38.01 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 591 113184.61 15.84 68.70 1.73- 1.26 591 86240.17 21.53 59.56 1.26- 1.09 591 59660.98 18.30 66.67 1.09- 0.96 591 55013.36 14.96 34.69 0.96- 0.88 591 17116.29 6.97 44.16 0.88- 0.80 591 50064.54 14.15 36.38 0.80- 0.76 591 18727.16 5.84 18.95 0.76- 0.71 591 20996.14 6.82 16.24 0.71- 0.67 591 24582.79 8.04 28.60 0.67- 0.63 592 3602.92 1.78 6.25 ------------------------------------------------------------------------------------ 6.00- 0.63 5911 44911.91 11.42 38.01 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:38:26 2019 Sorting 5911 observations 43 unique observations with > 7.00 F2/sig(F2) 5911 observations in 6 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 74 590 Total number of frames 590 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 14 frame = 1 scale 5911 observations in 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 5 46 Total number of frames 46 1425 observations > 7.00 F2/sig(F2) 1425 observations in 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 5 46 Total number of frames 46 Removing 'redundancy=1' reflections Average redundancy: 25.4 (Out of 1425 removed 2 = 1423, unique = 56) 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 6 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 5 46 Total number of frames 46 56 unique data precomputed (should be 56) 56 unique data with 1423 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 25.4 (Out of 1423 removed 0 = 1423, unique = 56) 56 unique data precomputed (should be 56) 56 unique data with 1423 observations RMS deviation of equivalent data = 0.31322 Rint = 0.26059 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.25137, wR= 0.34566 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13369, wR= 0.18995, Acormin=0.464, Acormax=1.411, Acor_av=1.002 F test: Probability=1.000, F= 3.523 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12244, wR= 0.17681, Acormin=0.441, Acormax=1.471, Acor_av=0.962 F test: Probability=0.999, F= 1.189 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12517, wR= 0.18000, Acormin=0.534, Acormax=1.530, Acor_av=0.998 F test: Probability=0.000, F= 0.953 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10904, wR= 0.16234, Acormin=0.412, Acormax=1.596, Acor_av=0.964 F test: Probability=1.000, F= 1.253 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09534, wR= 0.14805, Acormin=0.524, Acormax=1.813, Acor_av=1.006 F test: Probability=1.000, F= 1.301 Final absorption model (ne=4, no=3): Rint= 0.09534, Acormin=0.524, Acormax=1.813, Acor_av=1.006 Combined refinement in use Rint: 0.26235 There are 46 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 69 pars with 2415 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31322 Using Levenberg-Marquardt: 0.00010 New wR= 0.12255 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.26059 with corrections 0.09137 Rint for all data: 0.26235 with corrections 0.09398 2 observations identified as outliers and rejected Cycle 2 wR= 0.11206 Using Levenberg-Marquardt: 0.00001 New wR= 0.08792 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.26054 with corrections 0.05970 Rint for all data: 0.26235 with corrections 0.06558 2 observations identified as outliers and rejected Cycle 3 wR= 0.07941 Using Levenberg-Marquardt: 0.00000 New wR= 0.07536 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25973 with corrections 0.05430 Rint for all data: 0.26235 with corrections 0.06033 0 observations identified as outliers and rejected Cycle 4 wR= 0.07536 Using Levenberg-Marquardt: 0.00000 New wR= 0.07412 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25973 with corrections 0.05373 Rint for all data: 0.26235 with corrections 0.05962 0 observations identified as outliers and rejected Cycle 5 wR= 0.07412 Using Levenberg-Marquardt: 0.00000 New wR= 0.07364 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25973 with corrections 0.05351 Rint for all data: 0.26235 with corrections 0.05927 0 observations identified as outliers and rejected Final wR= 0.07364 Final frame scales: Min= 0.6965 Max= 1.2389 Final absorption correction factors: Amin= 0.3692 Amax= 1.6201 PROFFIT INFO: Inet (after scale3 abspack): min=-1077.4359 max=1277485.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=38.7361 max=22147.7148 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/104 5911 reflections read from tmp file 258 reflections are rejected (258 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 2 2 3 4 2 1 4 144 Initial Chi^2= 0.53137 Cycle 1, Chi^2= 1.00747 Current error model SIG(F2)^2 = 64.72*I_RAW + 10.86*I_BACK+(0.03719*)^2 Cycle 2, Chi^2= 1.01737 Current error model SIG(F2)^2 = 82.88*I_RAW + 6.26*I_BACK+(0.02852*)^2 Cycle 3, Chi^2= 1.01268 Current error model SIG(F2)^2 = 92.23*I_RAW + 4.42*I_BACK+(0.02521*)^2 Cycle 4, Chi^2= 1.00595 Current error model SIG(F2)^2 = 96.27*I_RAW + 3.75*I_BACK+(0.02426*)^2 Cycle 5, Chi^2= 1.00212 Current error model SIG(F2)^2 = 97.74*I_RAW + 3.54*I_BACK+(0.02402*)^2 Cycle 6, Chi^2= 1.00068 Current error model SIG(F2)^2 = 98.23*I_RAW + 3.47*I_BACK+(0.02396*)^2 Cycle 7, Chi^2= 1.00021 Current error model SIG(F2)^2 = 98.38*I_RAW + 3.45*I_BACK+(0.02394*)^2 Final Chi^2= 1.00021 Final error model SIG(F2)^2 = 98.38*I_RAW + 3.45*I_BACK+(0.02394*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1277486- 116690 591 378014.88 31.77 100.00 116650- 3461 591 28617.46 12.53 100.00 3452- 1991 591 2646.32 5.84 98.31 1991- 1145 591 1492.83 3.71 56.85 1145- 766 591 935.65 2.67 21.66 766- 514 591 634.64 2.31 13.20 514- 323 591 414.35 1.89 6.94 322- 149 591 238.17 1.48 3.21 149- 21 591 81.03 0.78 0.51 21- -1077 592 -131.79 -0.54 0.00 ------------------------------------------------------------------------------------ 1277486- -1077 5911 41287.35 6.24 40.06 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 591 105443.49 10.25 71.40 1.73- 1.26 591 79804.08 9.57 61.76 1.26- 1.09 591 54859.49 8.22 69.54 1.09- 0.96 591 49698.97 6.77 35.53 0.96- 0.88 591 15279.56 4.64 47.88 0.88- 0.80 591 46377.66 7.51 39.76 0.80- 0.76 591 17280.66 3.84 20.30 0.76- 0.71 591 18686.33 4.70 17.43 0.71- 0.67 591 22199.31 5.27 29.95 0.67- 0.63 592 3308.16 1.66 7.09 ------------------------------------------------------------------------------------ 6.00- 0.63 5911 41287.35 6.24 40.06 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 591 105443.49 10.25 71.40 6.00- 1.26 1182 92623.79 9.91 66.58 6.00- 1.09 1773 80035.69 9.35 67.57 6.00- 0.96 2364 72451.51 8.70 59.56 6.00- 0.88 2955 61017.12 7.89 57.23 6.00- 0.80 3546 58577.21 7.83 54.31 6.00- 0.76 4137 52677.70 7.26 49.46 6.00- 0.71 4728 48428.78 6.94 45.45 6.00- 0.67 5319 45514.40 6.75 43.73 6.00- 0.63 5911 41287.35 6.24 40.06 ------------------------------------------------------------------------------------ 6.00- 0.63 5911 41287.35 6.24 40.06 Scale applied to data: s=0.782787 (maximum obs:1277485.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.059; Rsigma 0.037: data 5911 -> merged 162 With outlier rejection... Rint 0.054; Rsigma 0.037: data 5898 -> merged 162 Rejected total: 13, method kkm 4, method Blessing 9 Completeness direct cell (a, b, c) = (10.411, 10.411, 10.411), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626653, 6.010641 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.41 - 1.76 14 14 38.71 100.00 542 1.74 - 1.27 14 14 42.43 100.00 594 1.26 - 1.06 14 14 47.93 100.00 671 1.05 - 0.97 14 14 41.71 100.00 584 0.95 - 0.88 14 14 43.29 100.00 606 0.87 - 0.81 14 14 38.43 100.00 538 0.80 - 0.76 14 14 40.50 100.00 567 0.76 - 0.72 14 14 33.86 100.00 474 0.72 - 0.69 14 14 37.36 100.00 523 0.69 - 0.65 19 19 31.16 100.00 592 --------------------------------------------------------------- 10.41 - 0.65 145 145 39.25 100.00 5691 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:38:25 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.407061 10.419285 10.405912 89.9842 89.9750 90.0170 5889 Reflections read from file xs2212a.hkl 5854 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.63 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2940 0 3882 3880 5854 N (int>3sigma) = 0 0 0 0 1331 0 1744 1728 2489 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 34.5 32.3 33.3 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.8 6.7 6.6 Lattice type: F chosen Volume: 1128.36 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.357 7.360 7.362 119.99 119.96 90.01 Niggli form: a.a = 54.124 b.b = 54.171 c.c = 54.196 b.c = -27.083 a.c = -27.043 a.b = -0.006 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.092 CUBIC F-lattice R(int) = 0.045 [ 5623] Vol = 1128.4 Cell: 10.419 10.407 10.406 89.97 90.02 89.98 Volume: 1128.36 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.091 TETRAGONAL I-lattice R(int) = 0.045 [ 5237] Vol = 564.2 Cell: 7.362 7.364 10.406 90.01 89.97 89.93 Volume: 564.18 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.055 TETRAGONAL I-lattice R(int) = 0.044 [ 5238] Vol = 564.2 Cell: 7.357 7.360 10.419 90.00 89.98 90.01 Volume: 564.18 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.075 TETRAGONAL I-lattice R(int) = 0.045 [ 5237] Vol = 564.2 Cell: 7.364 7.362 10.406 90.03 90.01 90.07 Volume: 564.18 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.061 ORTHORHOMBIC F-lattice R(int) = 0.044 [ 5184] Vol = 1128.4 Cell: 10.406 10.407 10.419 89.98 90.02 89.97 Volume: 1128.36 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.101 ORTHORHOMBIC I-lattice R(int) = 0.043 [ 5164] Vol = 564.2 Cell: 10.406 7.364 7.362 89.93 89.97 90.01 Volume: 564.18 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.020 ORTHORHOMBIC I-lattice R(int) = 0.043 [ 5166] Vol = 564.2 Cell: 7.357 7.360 10.419 90.00 90.02 90.01 Volume: 564.18 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.056 MONOCLINIC I-lattice R(int) = 0.042 [ 4639] Vol = 564.2 Cell: 7.362 10.406 7.364 90.01 90.07 90.03 Volume: 564.18 Matrix:-0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.056 MONOCLINIC I-lattice R(int) = 0.043 [ 4638] Vol = 564.2 Cell: 7.362 10.407 7.364 89.99 90.07 89.97 Volume: 564.18 Matrix: 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.049 MONOCLINIC I-lattice R(int) = 0.042 [ 4639] Vol = 564.2 Cell: 7.364 10.406 7.362 90.03 90.07 90.01 Volume: 564.18 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.006 MONOCLINIC I-lattice R(int) = 0.041 [ 4627] Vol = 564.2 Cell: 7.357 7.360 10.419 90.00 90.02 89.99 Volume: 564.18 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.016 MONOCLINIC I-lattice R(int) = 0.042 [ 4641] Vol = 564.2 Cell: 7.357 10.419 7.360 90.00 90.01 89.98 Volume: 564.18 Matrix: 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.039 MONOCLINIC I-lattice R(int) = 0.042 [ 4641] Vol = 564.2 Cell: 7.357 10.419 7.360 90.00 90.01 90.02 Volume: 564.18 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) = 0.037 [ 3583] Vol = 282.1 Cell: 7.357 7.360 7.362 119.99 119.96 90.01 Volume: 282.09 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -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 2940 0 3893 3899 5854 N (int>3sigma) = 0 0 0 0 1331 0 1765 1754 2489 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 32.8 34.3 33.3 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.7 6.8 6.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.424 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 39 39 423 1157 N I>3s 2 2 2 630 0.0 0.0 0.0 2.1 0.8 0.8 0.2 5.2 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 0.045 5228 Fd-3m 1 1 227 C N N N N 37 2284 0.045 5290 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.419285 10.407061 10.405912 89.9750 90.0158 89.9830 ZERR 5.00 0.001555 0.001328 0.001108 0.0096 0.0105 0.0112 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1126358- 88655 718 710 27 26.3 328455.10 29.66 0.050 0.065 76514- 1762 1118 1116 27 41.3 5210.35 7.87 0.091 0.107 1631- 757 1201 1199 27 44.4 1102.55 2.84 0.226 0.301 752- 314 1214 1213 27 44.9 479.55 1.93 0.369 0.513 307- 76 771 771 27 28.6 199.38 1.16 0.628 1.260 75- -133 889 889 27 32.9 15.93 0.22 0.967 4.356 ------------------------------------------------------------------------------------------- 1126358- -133 5911 5898 162 36.4 40876.47 6.22 0.054 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-1.27 1138 1134 27 42.0 94367.08 10.16 0.047 0.059 0.028 1.26-0.97 1221 1218 27 45.1 50572.32 7.31 0.049 0.062 0.033 0.97-0.81 1090 1087 27 40.3 33254.33 6.39 0.060 0.076 0.043 0.81-0.73 1062 1062 27 39.3 11013.70 3.15 0.072 0.093 0.064 0.73-0.67 882 881 27 32.6 25808.62 5.74 0.079 0.104 0.058 0.67-0.63 518 516 27 19.1 3679.55 1.74 0.132 0.106 0.135 ------------------------------------------------------------------------------------------------------ inf-0.63 5911 5898 162 36.4 40876.47 6.22 0.054 0.068 0.037 inf-0.65 5701 5689 144 39.5 42137.59 6.37 0.054 0.067 0.036 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-1.27 1134 27 27 100.0 42.0 94367.08 62.16 0.047 0.006 1.26-0.97 1218 27 27 100.0 45.1 50572.32 45.80 0.049 0.006 0.97-0.81 1087 27 27 100.0 40.3 33254.33 40.85 0.060 0.008 0.81-0.73 1062 27 27 100.0 39.3 11013.70 18.34 0.072 0.012 0.73-0.67 881 27 27 100.0 32.6 25808.62 33.55 0.079 0.011 0.67-0.63 516 27 27 100.0 19.1 3679.55 7.75 0.132 0.032 -------------------------------------------------------------------------------------------- inf-0.63 5898 162 162 100.0 36.4 40876.47 37.93 0.054 0.008 inf-0.65 5689 144 144 100.0 39.5 42137.59 39.10 0.054 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:45:26 2019) ID: 3668; threads 40; handles 811; mem 515508.00 (1204692.00)kB; time: 1w 5d 0h 56m 14s MEMORY INFO: Memory PF:224.0, Ph:556.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.4,peak PF: 700.2, WS: 471.6, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:226.0, Ph:558.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:505.2,peak PF: 700.2, WS: 473.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:45:26 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000014 0.000015 0.000014 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000013 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000016 0.000014 ) 10.42433 ( 0.00216 ) 10.43788 ( 0.00207 ) 10.40727 ( 0.00221 ) 89.88512 ( 0.01680 ) 89.79539 ( 0.01701 ) 90.20497 ( 0.01656 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:45:27 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000014 0.000015 0.000014 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000013 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000016 0.000014 ) M - matrix: 0.004643 0.000002 -0.000012 ( 0.000002 0.000001 0.000001 ) 0.000002 0.004634 -0.000002 ( 0.000001 0.000002 0.000001 ) -0.000012 -0.000002 0.004651 ( 0.000001 0.000001 0.000002 ) unit cell: 10.424(2) 10.438(2) 10.407(2) 89.885(17) 89.795(17) 90.205(17) V = 1132.4(4) unit cell: 10.4096(7) 10.4096(7) 10.4096(7) 90.0 90.0 90.0 V = 1127.98(12) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.938 ( 0.170) | 0.923 ( 0.398) | 1.01- 0.88 | 22 | 0.957 ( 0.073) | 1.004 ( 0.124) | 1.180 ( 0.493) | 0.88- 0.79 | 22 | 0.985 ( 0.059) | 1.028 ( 0.140) | 1.234 ( 0.387) | 0.79- 0.70 | 22 | 0.984 ( 0.041) | 0.962 ( 0.107) | 1.276 ( 0.475) | 0.70- 0.63 | 22 | 0.943 ( 0.038) | 0.917 ( 0.081) | 1.311 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 220 | 0.933 ( 0.193) | 0.943 ( 0.158) | 1.113 ( 0.914) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 251 peaks identified as outliers and rejected 251 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 251 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 251 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.933 ( 0.064) | 0.964 ( 0.109) | 0.868 ( 0.326) | 1.09- 0.91 | 25 | 0.958 ( 0.066) | 0.981 ( 0.099) | 1.061 ( 0.453) | 0.89- 0.82 | 25 | 0.934 ( 0.070) | 0.926 ( 0.093) | 1.119 ( 0.390) | 0.82- 0.72 | 25 | 0.952 ( 0.053) | 0.902 ( 0.085) | 1.407 ( 0.453) | 0.72- 0.63 | 26 | 0.928 ( 0.033) | 0.880 ( 0.090) | 1.365 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 251 | 0.920 ( 0.080) | 0.917 ( 0.119) | 1.055 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 251 obs out of 251 (total:251,skipped:0) (100.00%) UB - matrix: 0.066196 0.014133 0.006718 ( 0.000026 0.000034 0.000033 ) -0.015600 0.064667 0.012815 ( 0.000017 0.000022 0.000022 ) -0.003911 -0.014166 0.066843 ( 0.000023 0.000029 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004582 -0.000023 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000023 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.479(4) 10.371(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.6(7) OTKP changes: 251 1 1 1 OTKP changes: 251 1 1 1 No constraint UB - matrix: 0.066328 0.014183 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015580 0.064687 0.012854 ( 0.000017 0.000023 0.000022 ) -0.004072 -0.014197 0.066893 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004587 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066328 0.014183 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015580 0.064687 0.012854 ( 0.000017 0.000023 0.000022 ) -0.004072 -0.014197 0.066893 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 251 obs out of 251 (total:251,skipped:0) (100.00%) unit cell: 10.392(4) 10.473(3) 10.362(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.7(7) unit cell: 10.4088(5) 10.4088(5) 10.4088(5) 90.0 90.0 90.0 V = 1127.73(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.010) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066328 0.014183 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015580 0.064687 0.012854 ( 0.000017 0.000023 0.000022 ) -0.004072 -0.014197 0.066893 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004587 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066328 0.014183 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015580 0.064687 0.012854 ( 0.000017 0.000023 0.000022 ) -0.004072 -0.014197 0.066893 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 251 obs out of 251 (total:251,skipped:0) (100.00%) unit cell: 10.392(4) 10.473(3) 10.362(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.7(7) unit cell: 10.4088(5) 10.4088(5) 10.4088(5) 90.0 90.0 90.0 V = 1127.73(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 251 obs out of 251 (total:251,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 255 peaks identified as outliers and rejected 255 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 255 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 255 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 26 | 0.869 ( 0.088) | 0.876 ( 0.126) | 1.009 ( 0.497) | 2.37- 1.75 | 26 | 0.881 ( 0.097) | 0.900 ( 0.140) | 1.045 ( 0.533) | 1.75- 1.58 | 26 | 0.898 ( 0.094) | 0.880 ( 0.154) | 0.948 ( 0.391) | 1.58- 1.35 | 26 | 0.942 ( 0.084) | 0.962 ( 0.111) | 0.923 ( 0.446) | 1.35- 1.16 | 26 | 0.919 ( 0.075) | 0.921 ( 0.111) | 0.999 ( 0.581) | 1.16- 1.06 | 26 | 0.924 ( 0.071) | 0.963 ( 0.119) | 0.792 ( 0.261) | 1.06- 0.89 | 26 | 0.957 ( 0.065) | 0.970 ( 0.107) | 1.072 ( 0.459) | 0.89- 0.82 | 26 | 0.944 ( 0.071) | 0.928 ( 0.084) | 1.172 ( 0.407) | 0.79- 0.69 | 26 | 0.953 ( 0.048) | 0.916 ( 0.103) | 1.305 ( 0.463) | 0.69- 0.63 | 21 | 0.927 ( 0.036) | 0.869 ( 0.075) | 1.380 ( 0.452) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 255 | 0.921 ( 0.081) | 0.919 ( 0.121) | 1.058 ( 0.485) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb PROFFITPEAK info: 330 peaks in the peak location table UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 No constraint UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004618 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004618 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004618 ( 0.000000 0.000000 0.000001 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) unit cell: 10.4375(16) 10.4375(16) 10.4375(16) 90.0 90.0 90.0 V = 1137.1(3) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 199 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.156) HKL list info: 1283 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004618 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004618 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004618 ( 0.000000 0.000000 0.000001 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) unit cell: 10.4375(16) 10.4375(16) 10.4375(16) 90.0 90.0 90.0 V = 1137.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 192 peaks identified as outliers and rejected 192 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 192 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 192 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.97 | 19 | 0.842 ( 0.116) | 0.844 ( 0.171) | 0.956 ( 0.449) | 2.63- 1.84 | 19 | 0.822 ( 0.111) | 0.843 ( 0.187) | 0.847 ( 0.504) | 1.84- 1.59 | 19 | 0.842 ( 0.108) | 0.837 ( 0.164) | 0.836 ( 0.354) | 1.59- 1.36 | 19 | 0.936 ( 0.096) | 0.973 ( 0.144) | 0.805 ( 0.268) | 1.36- 1.20 | 19 | 0.950 ( 0.102) | 0.972 ( 0.160) | 0.845 ( 0.330) | 1.20- 1.01 | 19 | 0.995 ( 0.078) | 1.010 ( 0.137) | 1.101 ( 0.434) | 1.01- 0.88 | 19 | 0.998 ( 0.085) | 1.016 ( 0.121) | 1.030 ( 0.364) | 0.88- 0.79 | 19 | 1.037 ( 0.059) | 1.056 ( 0.123) | 0.938 ( 0.316) | 0.79- 0.72 | 19 | 1.031 ( 0.054) | 0.994 ( 0.144) | 1.279 ( 0.526) | 0.70- 0.63 | 21 | 0.975 ( 0.052) | 0.883 ( 0.059) | 1.164 ( 0.415) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 192 | 0.943 ( 0.117) | 0.942 ( 0.164) | 0.982 ( 0.432) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) UB - matrix: 0.065810 0.015591 0.006262 ( 0.000023 0.000019 0.000022 ) -0.016403 0.064531 0.013131 ( 0.000023 0.000020 0.000022 ) -0.002751 -0.014148 0.066421 ( 0.000026 0.000022 0.000025 ) M - matrix: 0.004608 0.000006 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004607 0.000005 ( 0.000002 0.000003 0.000002 ) 0.000014 0.000005 0.004623 ( 0.000002 0.000002 0.000003 ) unit cell: 10.450(3) 10.450(3) 10.432(4) 90.07(3) 90.17(3) 90.08(3) V = 1139.1(6) OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 1279 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 190 peaks identified as outliers and rejected 190 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 190 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 190 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 3.00 | 19 | 0.846 ( 0.114) | 0.847 ( 0.168) | 0.873 ( 0.501) | 2.99- 2.00 | 19 | 0.802 ( 0.108) | 0.800 ( 0.186) | 0.843 ( 0.452) | 1.84- 1.59 | 19 | 0.842 ( 0.097) | 0.828 ( 0.155) | 0.880 ( 0.351) | 1.59- 1.36 | 19 | 0.948 ( 0.083) | 0.983 ( 0.140) | 0.851 ( 0.258) | 1.36- 1.19 | 19 | 0.950 ( 0.094) | 0.960 ( 0.152) | 0.768 ( 0.211) | 1.19- 1.00 | 19 | 1.018 ( 0.060) | 1.041 ( 0.127) | 1.085 ( 0.364) | 1.00- 0.88 | 19 | 1.010 ( 0.085) | 1.031 ( 0.121) | 1.045 ( 0.373) | 0.88- 0.78 | 19 | 1.033 ( 0.056) | 1.044 ( 0.117) | 0.953 ( 0.322) | 0.78- 0.69 | 19 | 1.031 ( 0.055) | 1.004 ( 0.165) | 1.278 ( 0.531) | 0.69- 0.63 | 19 | 0.970 ( 0.050) | 0.876 ( 0.055) | 1.127 ( 0.364) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 190 | 0.945 ( 0.116) | 0.942 ( 0.169) | 0.970 ( 0.413) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.2 | 140 | 0.991 ( 0.040) | 1.036 ( 0.069) | 1.122 ( 0.499) | 10.2-14.9 | 140 | 0.995 ( 0.048) | 1.052 ( 0.071) | 1.096 ( 0.501) | 14.9-19.2 | 140 | 0.994 ( 0.181) | 1.034 ( 0.098) | 1.114 ( 0.952) | 19.3-23.6 | 140 | 0.970 ( 0.065) | 1.011 ( 0.086) | 0.949 ( 0.412) | 23.6-27.5 | 140 | 0.971 ( 0.070) | 1.008 ( 0.101) | 0.968 ( 0.453) | 27.6-32.7 | 140 | 0.943 ( 0.082) | 0.954 ( 0.104) | 0.943 ( 0.446) | 32.7-36.4 | 140 | 0.919 ( 0.156) | 0.907 ( 0.150) | 1.056 ( 0.656) | 36.4-39.0 | 140 | 0.892 ( 0.106) | 0.885 ( 0.246) | 1.010 ( 0.477) | 39.0-42.0 | 140 | 0.895 ( 0.106) | 0.838 ( 0.143) | 1.010 ( 0.451) | 42.0-50.1 | 137 | 0.868 ( 0.123) | 0.796 ( 0.141) | 0.931 ( 0.431) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 1397 | 0.944 ( 0.116) | 0.952 ( 0.156) | 1.020 ( 0.555) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.14 e2 dimension: a=-0.0069 b=1.24 e3 dimension: a=0.0004 b=1.10 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 4496 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385971 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 14:45:46 2019 PROFFITMAIN - Started at Wed Aug 21 14:45:46 2019 OTKP changes: 1085 2 5 6 OTKP changes: 1085 2 5 6 OTKP changes: 1085 2 5 6 No constraint UB - matrix: 0.066158 0.015082 0.006703 ( 0.000013 0.000014 0.000013 ) -0.016184 0.064858 0.013188 ( 0.000012 0.000013 0.000012 ) -0.003682 -0.014395 0.066588 ( 0.000014 0.000016 0.000015 ) M - matrix: 0.004652 0.000001 -0.000015 ( 0.000002 0.000001 0.000001 ) 0.000001 0.004641 -0.000002 ( 0.000001 0.000002 0.000001 ) -0.000015 -0.000002 0.004653 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066158 0.015082 0.006703 ( 0.000013 0.000014 0.000013 ) -0.016184 0.064858 0.013188 ( 0.000012 0.000013 0.000012 ) -0.003682 -0.014395 0.066588 ( 0.000014 0.000016 0.000015 ) M - matrix: 0.004649 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004649 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004649 ( 0.000000 0.000000 0.000001 ) UB fit with 1115 obs out of 1397 (total:1397,skipped:0) (79.81%) unit cell: 10.399(2) 10.411(2) 10.399(2) 89.975(17) 89.813(17) 90.014(16) V = 1125.9(4) unit cell: 10.4030(7) 10.4030(7) 10.4030(7) 90.0 90.0 90.0 V = 1125.85(13) *** 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 187 obs out of 220 (total:220,skipped:0) (85.00%) UB - matrix: 0.066500 0.011702 0.008960 ( 0.000032 0.000043 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000030 0.000040 0.000034 ) -0.006052 -0.013931 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.60(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004603 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 220 (total:220,skipped:0) (85.91%) unit cell: 10.406(5) 10.502(6) 10.456(6) 90.61(5) 90.19(4) 89.64(4) V = 1143(1) unit cell: 10.4543(19) 10.4543(19) 10.4543(19) 90.0 90.0 90.0 V = 1142.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 220 (total:220,skipped:0) (92.27%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004644 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 220 (total:220,skipped:0) (93.64%) unit cell: 10.409(4) 10.492(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1140.0(9) unit cell: 10.4466(13) 10.4466(13) 10.4466(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) UB - matrix: 0.066334 0.014185 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015587 0.064701 0.012865 ( 0.000017 0.000023 0.000023 ) -0.004067 -0.014194 0.066894 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000010 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000010 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004686 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.471(3) 10.362(4) 89.74(3) 89.72(3) 89.88(3) V = 1127.3(7) OTKP changes: 255 1 1 1 OTKP changes: 255 1 1 1 No constraint UB - matrix: 0.066324 0.014177 0.006770 ( 0.000027 0.000035 0.000035 ) -0.015569 0.064673 0.012872 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014198 0.066868 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004658 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004585 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004683 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066324 0.014177 0.006770 ( 0.000027 0.000035 0.000035 ) -0.015569 0.064673 0.012872 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014198 0.066868 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) unit cell: 10.393(4) 10.475(3) 10.365(4) 89.74(3) 89.71(3) 89.89(3) V = 1128.4(7) unit cell: 10.4110(5) 10.4110(5) 10.4110(5) 90.0 90.0 90.0 V = 1128.44(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.030) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066324 0.014177 0.006770 ( 0.000027 0.000035 0.000035 ) -0.015569 0.064673 0.012872 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014198 0.066868 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004658 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004585 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004683 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066324 0.014177 0.006770 ( 0.000027 0.000035 0.000035 ) -0.015569 0.064673 0.012872 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014198 0.066868 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) unit cell: 10.393(4) 10.475(3) 10.365(4) 89.74(3) 89.71(3) 89.89(3) V = 1128.4(7) unit cell: 10.4110(5) 10.4110(5) 10.4110(5) 90.0 90.0 90.0 V = 1128.44(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068221 -0.000102 -0.000274 ( 0.000020 0.000026 0.000026 ) 0.000025 0.067866 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 0.000001 0.068348 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004654 -0.000005 -0.000019 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004606 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000019 -0.000011 0.004671 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068221 -0.000102 -0.000274 ( 0.000020 0.000026 0.000026 ) 0.000025 0.067866 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 0.000001 0.068348 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) unit cell: 10.397(3) 10.452(3) 10.378(3) 89.86(2) 89.76(2) 89.93(3) V = 1127.7(6) unit cell: 10.4088(5) 10.4088(5) 10.4088(5) 90.0 90.0 90.0 V = 1127.71(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065885 0.015206 0.006810 ( 0.000019 0.000013 0.000019 ) -0.016068 0.064789 0.013229 ( 0.000017 0.000012 0.000017 ) -0.003636 -0.014505 0.066501 ( 0.000021 0.000015 0.000021 ) M - matrix: 0.004612 0.000014 -0.000006 ( 0.000003 0.000001 0.000002 ) 0.000014 0.004639 -0.000004 ( 0.000001 0.000002 0.000002 ) -0.000006 -0.000004 0.004644 ( 0.000002 0.000002 0.000003 ) unit cell: 10.444(3) 10.414(2) 10.409(3) 89.952(19) 89.93(2) 90.168(19) V = 1132.1(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065946 0.015233 0.006782 ( 0.000020 0.000014 0.000019 ) -0.016129 0.064858 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003635 -0.014462 0.066588 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004622 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004648 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004656 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065946 0.015233 0.006782 ( 0.000020 0.000014 0.000019 ) -0.016129 0.064858 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003635 -0.014462 0.066588 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.433(3) 10.4043(19) 10.395(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.4(5) unit cell: 10.4108(5) 10.4108(5) 10.4108(5) 90.0 90.0 90.0 V = 1128.39(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.019) HKL list info: 1275 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065946 0.015233 0.006782 ( 0.000020 0.000014 0.000019 ) -0.016129 0.064858 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003635 -0.014462 0.066588 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004622 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004648 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004656 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065946 0.015233 0.006782 ( 0.000020 0.000014 0.000019 ) -0.016129 0.064858 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003635 -0.014462 0.066588 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.433(3) 10.4043(19) 10.395(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.4(5) unit cell: 10.4108(5) 10.4108(5) 10.4108(5) 90.0 90.0 90.0 V = 1128.39(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065946 0.015233 0.006782 ( 0.000020 0.000014 0.000019 ) -0.016129 0.064858 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003635 -0.014462 0.066588 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004622 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004648 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004656 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065946 0.015233 0.006782 ( 0.000020 0.000014 0.000019 ) -0.016129 0.064858 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003635 -0.014462 0.066588 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.433(3) 10.4043(19) 10.395(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.4(5) unit cell: 10.4108(5) 10.4108(5) 10.4108(5) 90.0 90.0 90.0 V = 1128.39(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066119 0.015253 0.006582 ( 0.000015 0.000020 0.000017 ) -0.016339 0.064737 0.012925 ( 0.000012 0.000016 0.000013 ) -0.003350 -0.014202 0.066521 ( 0.000011 0.000014 0.000012 ) M - matrix: 0.004650 -0.000002 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000002 0.004625 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.004635 ( 0.000001 0.000001 0.000002 ) unit cell: 10.402(2) 10.429(2) 10.4180(19) 89.906(16) 90.014(17) 89.980(19) V = 1130.2(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066165 0.015278 0.006523 ( 0.000013 0.000018 0.000015 ) -0.016373 0.064800 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003341 -0.014170 0.066624 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004657 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004633 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066165 0.015278 0.006523 ( 0.000013 0.000018 0.000015 ) -0.016373 0.064800 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003341 -0.014170 0.066624 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.394(2) 10.420(2) 10.4025(18) 89.945(16) 89.960(15) 89.965(18) V = 1126.7(4) unit cell: 10.4056(5) 10.4056(5) 10.4056(5) 90.0 90.0 90.0 V = 1126.68(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.019) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066165 0.015278 0.006523 ( 0.000013 0.000018 0.000015 ) -0.016373 0.064800 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003341 -0.014170 0.066624 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004657 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004633 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066165 0.015278 0.006523 ( 0.000013 0.000018 0.000015 ) -0.016373 0.064800 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003341 -0.014170 0.066624 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.394(2) 10.420(2) 10.4025(18) 89.945(16) 89.960(15) 89.965(18) V = 1126.7(4) unit cell: 10.4056(5) 10.4056(5) 10.4056(5) 90.0 90.0 90.0 V = 1126.68(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068227 -0.000037 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068083 -0.000054 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068188 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004655 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004635 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004650 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068227 -0.000037 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068083 -0.000054 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068188 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.3962(16) 10.418(3) 10.4021(15) 89.963(16) 89.976(13) 89.969(17) V = 1126.6(4) unit cell: 10.4055(5) 10.4055(5) 10.4055(5) 90.0 90.0 90.0 V = 1126.65(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 255 obs out of 271 (total:271,skipped:0) (94.10%) UB - matrix: 0.065959 0.015324 0.006331 ( 0.000017 0.000012 0.000013 ) -0.016394 0.064813 0.013400 ( 0.000021 0.000015 0.000016 ) -0.003060 -0.014525 0.066487 ( 0.000027 0.000020 0.000020 ) M - matrix: 0.004629 -0.000007 -0.000006 ( 0.000002 0.000002 0.000002 ) -0.000007 0.004647 -0.000000 ( 0.000002 0.000002 0.000002 ) -0.000006 -0.000000 0.004640 ( 0.000002 0.000002 0.000003 ) unit cell: 10.426(2) 10.406(2) 10.413(3) 90.00(2) 89.93(2) 89.91(2) V = 1129.6(5) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.066061 0.015393 0.006338 ( 0.000016 0.000012 0.000013 ) -0.016403 0.064860 0.013375 ( 0.000018 0.000014 0.000014 ) -0.002880 -0.014634 0.066577 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004641 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004658 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004651 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066061 0.015393 0.006338 ( 0.000016 0.000012 0.000013 ) -0.016403 0.064860 0.013375 ( 0.000018 0.000014 0.000014 ) -0.002880 -0.014634 0.066577 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.411(2) 10.393(2) 10.4000(18) 89.886(15) 90.093(17) 89.940(18) V = 1125.3(4) unit cell: 10.4014(5) 10.4014(5) 10.4014(5) 90.0 90.0 90.0 V = 1125.32(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.019) HKL list info: 1297 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066061 0.015393 0.006338 ( 0.000016 0.000012 0.000013 ) -0.016403 0.064860 0.013375 ( 0.000018 0.000014 0.000014 ) -0.002880 -0.014634 0.066577 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004641 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004658 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004651 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066061 0.015393 0.006338 ( 0.000016 0.000012 0.000013 ) -0.016403 0.064860 0.013375 ( 0.000018 0.000014 0.000014 ) -0.002880 -0.014634 0.066577 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.411(2) 10.393(2) 10.4000(18) 89.886(15) 90.093(17) 89.940(18) V = 1125.3(4) unit cell: 10.4014(5) 10.4014(5) 10.4014(5) 90.0 90.0 90.0 V = 1125.32(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068132 -0.000096 0.000072 ( 0.000017 0.000013 0.000014 ) 0.000060 0.068218 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068195 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004642 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004654 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004651 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068132 -0.000096 0.000072 ( 0.000017 0.000013 0.000014 ) 0.000060 0.068218 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068195 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.411(3) 10.3976(16) 10.4011(18) 89.930(13) 90.044(17) 89.970(16) V = 1125.9(4) unit cell: 10.4031(5) 10.4031(5) 10.4031(5) 90.0 90.0 90.0 V = 1125.88(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) UB - matrix: 0.066047 0.015581 0.006343 ( 0.000019 0.000015 0.000018 ) -0.016416 0.064702 0.013085 ( 0.000022 0.000019 0.000022 ) -0.002863 -0.014361 0.066612 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004640 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004635 -0.000011 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000011 0.004649 ( 0.000002 0.000002 0.000002 ) unit cell: 10.413(3) 10.418(3) 10.403(2) 89.86(2) 90.17(2) 90.10(2) V = 1128.6(5) OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 1266 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066047 0.015581 0.006343 ( 0.000019 0.000015 0.000018 ) -0.016416 0.064702 0.013085 ( 0.000022 0.000019 0.000022 ) -0.002863 -0.014361 0.066612 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004640 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004635 -0.000011 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000011 0.004649 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066047 0.015581 0.006343 ( 0.000019 0.000015 0.000018 ) -0.016416 0.064702 0.013085 ( 0.000022 0.000019 0.000022 ) -0.002863 -0.014361 0.066612 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.413(3) 10.418(3) 10.403(2) 89.86(2) 90.17(2) 90.10(2) V = 1128.6(5) unit cell: 10.4114(7) 10.4114(7) 10.4114(7) 90.0 90.0 90.0 V = 1128.57(12) 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! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: 0.068144 0.000081 0.000193 ( 0.000019 0.000016 0.000019 ) -0.000012 0.068090 -0.000152 ( 0.000021 0.000017 0.000020 ) -0.000002 -0.000000 0.068177 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004644 0.000005 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000005 0.004636 -0.000010 ( 0.000002 0.000002 0.000002 ) 0.000013 -0.000010 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.068144 0.000081 0.000193 ( 0.000019 0.000016 0.000019 ) -0.000012 0.068090 -0.000152 ( 0.000021 0.000017 0.000020 ) -0.000002 -0.000000 0.068177 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.409(3) 10.417(3) 10.4039(18) 89.873(19) 90.161(19) 90.06(2) V = 1128.1(5) unit cell: 10.4099(7) 10.4099(7) 10.4099(7) 90.0 90.0 90.0 V = 1128.09(12) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068158 0.000019 -0.000048 ( 0.000009 0.000009 0.000009 ) -0.000002 0.068099 0.000001 ( 0.000009 0.000010 0.000010 ) 0.000026 -0.000016 0.068177 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004645 0.000001 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000001 0.004637 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000001 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068158 0.000019 -0.000048 ( 0.000009 0.000009 0.000009 ) -0.000002 0.068099 0.000001 ( 0.000009 0.000010 0.000010 ) 0.000026 -0.000016 0.068177 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 1373 obs out of 1397 (total:1397,skipped:0) (98.28%) unit cell: 10.4067(13) 10.4157(15) 10.4038(11) 89.987(10) 89.981(9) 90.014(11) V = 1127.7(2) unit cell: 10.4087(3) 10.4087(3) 10.4087(3) 90.0 90.0 90.0 V = 1127.70(6) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 154 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof 6139 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:45:56 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.030) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.019) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.019) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.019) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) PROFFIT INFO: signal sum: min=-775.0000 max=7911026.0000 PROFFIT INFO: signal sum lp corr: min=-739.4975 max=1267836.8077 PROFFIT INFO: background sum: min=-100.0000 max=8226.0000 PROFFIT INFO: background sum sig2: min=423.0000 max=5841.0000 PROFFIT INFO: num of signal pixels: min=41 max=517 PROFFIT INFO: Inet: min=-1183.1959 max=2028538.8750 PROFFIT INFO: sig(Inet): min=51.9750 max=30729.5449 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=276.56 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 544 2112 3201 3810 4108 4762 5174 5433 5816 6073 6139 Percent 8.9 34.4 52.1 62.1 66.9 77.6 84.3 88.5 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 6139 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 6139 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2028539- 129245 613 413250.14 77.86 100.00 129237- 4054 613 29506.19 19.66 100.00 4051- 2047 613 2872.91 7.11 97.06 2045- 1225 613 1582.68 3.93 52.69 1225- 814 613 1001.60 2.32 15.66 813- 543 613 669.09 1.74 8.65 542- 338 613 433.35 1.22 5.22 338- 152 613 243.29 0.72 0.65 152- 18 613 80.57 0.29 0.00 18- -1183 622 -130.07 -0.25 0.00 ------------------------------------------------------------------------------------ 2028539- -1183 6139 44884.89 11.44 37.94 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 613 113660.59 15.98 69.33 1.73- 1.26 613 85269.52 21.27 59.05 1.26- 1.09 613 61580.33 18.94 67.70 1.09- 0.96 613 53980.31 14.72 33.61 0.96- 0.88 613 17318.14 7.09 43.72 0.88- 0.81 613 50327.72 14.18 36.70 0.80- 0.76 613 18363.99 5.73 18.11 0.76- 0.71 613 21182.54 6.93 16.97 0.71- 0.67 613 24179.39 7.95 28.55 0.67- 0.63 622 3592.58 1.77 6.11 ------------------------------------------------------------------------------------ 6.00- 0.63 6139 44884.89 11.44 37.94 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:45:56 2019 Sorting 6139 observations 53 unique observations with > 7.00 F2/sig(F2) 6139 observations in 6 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 Total number of frames 614 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 12 frame = 1 scale 6139 observations in 6 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 6 0 8 54 Total number of frames 54 1480 observations > 7.00 F2/sig(F2) 1480 observations in 6 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 6 0 8 54 Total number of frames 54 Removing 'redundancy=1' reflections Average redundancy: 22.0 (Out of 1480 removed 7 = 1473, unique = 67) 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 1473 observations in 6 runs Run # start # end # total # 1 0 8 9 2 0 8 18 3 0 8 27 4 0 8 36 5 0 8 45 6 0 8 54 Total number of frames 54 67 unique data precomputed (should be 67) 67 unique data with 1473 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.0 (Out of 1473 removed 0 = 1473, unique = 67) 67 unique data precomputed (should be 67) 67 unique data with 1473 observations RMS deviation of equivalent data = 0.31097 Rint = 0.25630 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24734, wR= 0.33829 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13196, wR= 0.18690, Acormin=0.459, Acormax=1.408, Acor_av=1.002 F test: Probability=1.000, F= 3.500 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12126, wR= 0.17383, Acormin=0.446, Acormax=1.466, Acor_av=0.969 F test: Probability=0.999, F= 1.182 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12633, wR= 0.17771, Acormin=0.540, Acormax=1.521, Acor_av=0.997 F test: Probability=0.000, F= 0.917 Trying model 4 (ne=4, no=1)... Results: Rint= 0.11003, wR= 0.16064, Acormin=0.429, Acormax=1.573, Acor_av=0.971 F test: Probability=1.000, F= 1.207 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09552, wR= 0.14606, Acormin=0.525, Acormax=1.807, Acor_av=1.012 F test: Probability=1.000, F= 1.320 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11868, wR= 0.16906, Acormin=0.403, Acormax=1.590, Acor_av=0.971 F test: Probability=0.000, F= 0.646 Trying model 7 (ne=6, no=1)... Results: Rint= 0.10544, wR= 0.15463, Acormin=0.402, Acormax=1.638, Acor_av=0.957 F test: Probability=0.000, F= 0.817 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09276, wR= 0.14255, Acormin=0.471, Acormax=1.774, Acor_av=0.990 F test: Probability=0.819, F= 1.050 Trying model 9 (ne=6, no=5)... Results: Rint= 0.14575, wR= 0.18776, Acormin=0.104, Acormax=1.001, Acor_av=0.515 F test: Probability=0.000, F= 0.422 Final absorption model (ne=4, no=3): Rint= 0.09552, Acormin=0.525, Acormax=1.807, Acor_av=1.012 Combined refinement in use Rint: 0.25806 There are 54 active scales (one needs to be fixed) Refinement control: frame scale #41 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 77 pars with 3003 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31097 Using Levenberg-Marquardt: 0.00010 New wR= 0.10893 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25630 with corrections 0.07847 Rint for all data: 0.25806 with corrections 0.08119 3 observations identified as outliers and rejected Cycle 2 wR= 0.09935 Using Levenberg-Marquardt: 0.00001 New wR= 0.08286 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25611 with corrections 0.05598 Rint for all data: 0.25806 with corrections 0.06172 2 observations identified as outliers and rejected Cycle 3 wR= 0.07672 Using Levenberg-Marquardt: 0.00000 New wR= 0.07411 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25536 with corrections 0.05171 Rint for all data: 0.25806 with corrections 0.05803 1 observations identified as outliers and rejected Cycle 4 wR= 0.07005 Using Levenberg-Marquardt: 0.00000 New wR= 0.06954 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25405 with corrections 0.04788 Rint for all data: 0.25806 with corrections 0.05495 1 observations identified as outliers and rejected Cycle 5 wR= 0.06697 Using Levenberg-Marquardt: 0.00000 New wR= 0.06573 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25386 with corrections 0.04639 Rint for all data: 0.25806 with corrections 0.05381 0 observations identified as outliers and rejected Final wR= 0.06573 Final frame scales: Min= 0.6407 Max= 1.3686 Final absorption correction factors: Amin= 0.3703 Amax= 1.6086 PROFFIT INFO: Inet (after scale3 abspack): min=-1115.4717 max=1241774.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=37.3552 max=24302.0996 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/104 6139 reflections read from tmp file 209 reflections are rejected (208 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 2 5 3 5 7 1 4 210 Initial Chi^2= 0.52373 Cycle 1, Chi^2= 1.01925 Current error model SIG(F2)^2 = 63.34*I_RAW + 10.68*I_BACK+(0.03384*)^2 Cycle 2, Chi^2= 1.01927 Current error model SIG(F2)^2 = 79.44*I_RAW + 6.76*I_BACK+(0.02688*)^2 Cycle 3, Chi^2= 1.01035 Current error model SIG(F2)^2 = 86.75*I_RAW + 5.40*I_BACK+(0.02453*)^2 Cycle 4, Chi^2= 1.00416 Current error model SIG(F2)^2 = 89.64*I_RAW + 4.93*I_BACK+(0.02386*)^2 Cycle 5, Chi^2= 1.00144 Current error model SIG(F2)^2 = 90.66*I_RAW + 4.78*I_BACK+(0.02368*)^2 Cycle 6, Chi^2= 1.00047 Current error model SIG(F2)^2 = 91.00*I_RAW + 4.73*I_BACK+(0.02362*)^2 Cycle 7, Chi^2= 1.00015 Current error model SIG(F2)^2 = 91.10*I_RAW + 4.71*I_BACK+(0.02361*)^2 Final Chi^2= 1.00015 Final error model SIG(F2)^2 = 91.10*I_RAW + 4.71*I_BACK+(0.02361*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1241774- 117397 613 376485.31 32.64 100.00 116959- 3374 613 29199.89 13.04 100.00 3371- 2011 613 2642.53 6.06 99.02 2010- 1143 613 1497.21 3.85 61.83 1139- 759 613 932.04 2.71 25.45 759- 512 613 636.27 2.36 14.03 512- 321 613 412.40 1.95 8.97 321- 148 613 235.96 1.46 2.94 148- 17 613 78.58 0.75 0.49 17- -1115 622 -129.74 -0.55 0.00 ------------------------------------------------------------------------------------ 1241774- -1115 6139 41138.45 6.42 41.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 613 105634.68 10.64 72.43 1.73- 1.26 613 77946.35 9.73 61.83 1.26- 1.09 613 56780.56 8.65 71.29 1.09- 0.96 613 48750.16 6.83 35.40 0.96- 0.88 613 16055.49 4.85 49.43 0.88- 0.81 613 45848.51 7.72 42.25 0.80- 0.76 613 16819.25 3.87 20.88 0.76- 0.71 613 19006.50 4.90 20.07 0.71- 0.67 613 21804.55 5.38 31.48 0.67- 0.63 622 3294.13 1.67 7.56 ------------------------------------------------------------------------------------ 6.00- 0.63 6139 41138.45 6.42 41.21 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 613 105634.68 10.64 72.43 6.00- 1.26 1226 91790.51 10.19 67.13 6.00- 1.09 1839 80120.53 9.67 68.52 6.00- 0.96 2452 72277.94 8.96 60.24 6.00- 0.88 3065 61033.45 8.14 58.08 6.00- 0.81 3678 58502.62 8.07 55.44 6.00- 0.76 4291 52547.86 7.47 50.50 6.00- 0.71 4904 48355.19 7.15 46.70 6.00- 0.67 5517 45405.12 6.95 45.01 6.00- 0.63 6139 41138.45 6.42 41.21 ------------------------------------------------------------------------------------ 6.00- 0.63 6139 41138.45 6.42 41.21 Scale applied to data: s=0.805298 (maximum obs:1241774.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.054; Rsigma 0.036: data 6139 -> merged 240 With outlier rejection... Rint 0.048; Rsigma 0.036: data 6117 -> merged 240 Rejected total: 22, method kkm 12, method Blessing 10 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626533, 6.009493 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.42 - 1.59 21 21 33.67 100.00 707 1.57 - 1.20 21 21 34.57 100.00 726 1.19 - 1.02 21 21 32.71 100.00 687 1.02 - 0.91 21 21 31.29 100.00 657 0.91 - 0.84 21 21 27.81 100.00 584 0.84 - 0.78 21 21 27.24 100.00 572 0.78 - 0.74 21 21 25.81 100.00 542 0.74 - 0.71 21 21 21.86 100.00 459 0.71 - 0.68 21 21 24.14 100.00 507 0.68 - 0.65 23 23 20.30 100.00 467 --------------------------------------------------------------- 10.42 - 0.65 212 212 27.87 100.00 5908 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:45:57 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.406731 10.415745 10.403771 89.9867 89.9811 90.0143 6117 Reflections read from file xs2212a.hkl 6084 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3052 0 4041 4033 6084 N (int>3sigma) = 0 0 0 0 1332 0 1774 1745 2514 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 34.3 32.2 32.9 Mean int/sigma = 0.0 0.0 0.0 0.0 3.9 0.0 6.6 6.4 6.4 Lattice type: F chosen Volume: 1127.70 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.356 7.359 7.360 119.99 119.96 90.02 Niggli form: a.a = 54.117 b.b = 54.152 c.c = 54.169 b.c = -27.069 a.c = -27.038 a.b = -0.015 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.087 CUBIC F-lattice R(int) = 0.048 [ 5853] Vol = 1127.7 Cell: 10.416 10.407 10.404 89.98 90.01 89.99 Volume: 1127.70 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.067 TETRAGONAL I-lattice R(int) = 0.047 [ 5467] Vol = 563.9 Cell: 7.361 7.363 10.404 90.00 89.98 89.95 Volume: 563.85 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.045 TETRAGONAL I-lattice R(int) = 0.047 [ 5467] Vol = 563.9 Cell: 7.356 7.359 10.416 90.00 89.98 90.02 Volume: 563.85 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.056 TETRAGONAL I-lattice R(int) = 0.047 [ 5467] Vol = 563.9 Cell: 7.363 7.361 10.404 90.02 90.00 90.05 Volume: 563.85 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.047 ORTHORHOMBIC F-lattice R(int) = 0.047 [ 5415] Vol = 1127.7 Cell: 10.404 10.407 10.416 89.99 90.01 89.98 Volume: 1127.70 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.074 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 5394] Vol = 563.9 Cell: 10.404 7.363 7.361 89.95 89.98 90.00 Volume: 563.85 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.027 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 5397] Vol = 563.9 Cell: 7.356 7.359 10.416 90.00 90.02 90.02 Volume: 563.85 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.043 MONOCLINIC I-lattice R(int) = 0.044 [ 4870] Vol = 563.9 Cell: 7.361 10.404 7.363 90.00 90.05 90.02 Volume: 563.85 Matrix:-0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.043 MONOCLINIC I-lattice R(int) = 0.045 [ 4868] Vol = 563.9 Cell: 7.360 10.407 7.362 90.00 90.07 89.98 Volume: 563.85 Matrix: 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.037 MONOCLINIC I-lattice R(int) = 0.044 [ 4870] Vol = 563.9 Cell: 7.363 10.404 7.361 90.02 90.05 90.00 Volume: 563.85 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.017 MONOCLINIC I-lattice R(int) = 0.044 [ 4858] Vol = 563.9 Cell: 7.356 7.359 10.416 90.00 90.02 89.98 Volume: 563.85 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.013 MONOCLINIC I-lattice R(int) = 0.044 [ 4871] Vol = 563.9 Cell: 7.356 10.416 7.359 90.00 90.02 89.98 Volume: 563.85 Matrix: 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.033 MONOCLINIC I-lattice R(int) = 0.044 [ 4871] Vol = 563.9 Cell: 7.356 10.416 7.359 90.00 90.02 90.02 Volume: 563.85 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 [ 3811] Vol = 281.9 Cell: 7.356 7.359 7.360 119.99 119.96 90.02 Volume: 281.93 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -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 3052 0 4045 4047 6084 N (int>3sigma) = 0 0 0 0 1332 0 1784 1771 2514 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 32.7 33.7 32.9 Mean int/sigma = 0.0 0.0 0.0 0.0 3.9 0.0 6.5 6.5 6.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.449 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 42 42 454 1199 N I>3s 2 2 2 636 0.0 0.0 0.0 2.0 0.8 0.8 0.2 5.0 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 0.048 5427 Fd-3m 1 1 227 C N N N N 37 2284 0.048 5489 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415745 10.406731 10.403771 89.9811 90.0133 89.9857 ZERR 5.00 0.001473 0.001328 0.001068 0.0095 0.0101 0.0109 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1131867- 125330 613 603 26 23.2 376511.54 32.66 0.043 0.055 105962- 3068 692 688 26 26.5 26415.34 12.18 0.067 0.080 2972- 1361 892 889 26 34.2 2182.46 5.47 0.125 0.181 1343- 853 771 771 26 29.7 1033.40 2.71 0.237 0.308 802- 492 752 752 26 28.9 633.08 2.28 0.302 0.415 487- 296 744 743 26 28.6 380.05 1.75 0.446 0.618 295- 136 560 559 26 21.5 221.17 1.30 0.576 0.982 133- 31 591 590 26 22.7 71.94 0.55 0.885 2.308 21- -186 524 522 32 16.3 -28.58 -0.06 0.989 4.143 ------------------------------------------------------------------------------------------- 1131867- -186 6139 6117 240 25.5 40682.82 6.38 0.048 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-1.44 905 901 26 34.7 113950.27 11.69 0.042 0.051 0.026 1.39-1.09 937 934 26 35.9 44935.06 7.58 0.045 0.058 0.032 1.06-0.94 784 781 26 30.0 37894.60 5.85 0.043 0.054 0.035 0.92-0.84 744 743 26 28.6 41246.02 7.64 0.048 0.064 0.040 0.84-0.78 725 722 26 27.8 23413.62 5.01 0.054 0.068 0.047 0.78-0.73 619 618 26 23.8 8462.55 3.11 0.077 0.096 0.075 0.73-0.69 646 646 27 23.9 18812.63 4.65 0.067 0.085 0.061 0.68-0.66 559 556 27 20.6 14268.41 3.82 0.080 0.112 0.068 0.65-0.63 220 216 30 7.2 8130.04 2.44 0.087 0.085 0.085 ------------------------------------------------------------------------------------------------------ inf-0.63 6139 6117 240 25.5 40682.82 6.38 0.048 0.061 0.036 inf-0.65 5924 5906 211 28.0 41916.44 6.54 0.047 0.060 0.036 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-1.44 901 26 26 100.0 34.7 113950.27 68.71 0.042 0.006 1.39-1.09 934 26 26 100.0 35.9 44935.06 41.18 0.045 0.007 1.06-0.94 781 26 26 100.0 30.0 37894.60 33.01 0.043 0.007 0.92-0.84 743 26 26 100.0 28.6 41246.02 40.44 0.048 0.008 0.84-0.78 722 26 26 100.0 27.8 23413.62 24.92 0.054 0.009 0.78-0.73 618 26 26 100.0 23.8 8462.55 15.28 0.077 0.016 0.73-0.69 646 27 27 100.0 23.9 18812.63 21.52 0.067 0.013 0.68-0.66 556 27 27 100.0 20.6 14268.41 18.70 0.080 0.015 0.65-0.63 216 30 30 100.0 7.2 8130.04 6.30 0.087 0.034 -------------------------------------------------------------------------------------------- inf-0.63 6117 240 240 100.0 25.5 40682.82 34.22 0.048 0.008 inf-0.65 5906 211 211 100.0 28.0 41916.44 35.25 0.047 0.008 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066113 0.015077 0.006857 ( 0.000009 0.000009 0.000009 ) -0.016164 0.064822 0.013192 ( 0.000009 0.000010 0.000010 ) -0.003628 -0.014421 0.066536 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004645 0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.004637 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000001 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066113 0.015077 0.006857 ( 0.000009 0.000009 0.000009 ) -0.016164 0.064822 0.013192 ( 0.000009 0.000010 0.000010 ) -0.003628 -0.014421 0.066536 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4069(13) 10.4160(15) 10.4038(11) 89.988(10) 89.984(9) 90.016(11) V = 1127.8(2) unit cell: 10.4089(3) 10.4089(3) 10.4089(3) 90.0 90.0 90.0 V = 1127.76(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.030) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.019) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.019) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.019) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) PROFFIT INFO: signal sum: min=-775.0000 max=7911026.0000 PROFFIT INFO: signal sum lp corr: min=-739.4975 max=1267836.8077 PROFFIT INFO: background sum: min=-100.0000 max=8226.0000 PROFFIT INFO: background sum sig2: min=423.0000 max=5841.0000 PROFFIT INFO: num of signal pixels: min=41 max=517 PROFFIT INFO: Inet: min=-1183.1959 max=2028538.8750 PROFFIT INFO: sig(Inet): min=51.9750 max=30729.5449 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=276.56 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 1088 4224 6402 7620 8216 9524 10348 10866 11632 12146 12278 Percent 8.9 34.4 52.1 62.1 66.9 77.6 84.3 88.5 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 6139 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 6139 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2028539- 129245 613 413250.14 77.86 100.00 129237- 4054 613 29506.19 19.66 100.00 4051- 2047 613 2872.91 7.11 97.06 2045- 1225 613 1582.68 3.93 52.69 1225- 814 613 1001.60 2.32 15.66 813- 543 613 669.09 1.74 8.65 542- 338 613 433.35 1.22 5.22 338- 152 613 243.29 0.72 0.65 152- 18 613 80.57 0.29 0.00 18- -1183 622 -130.07 -0.25 0.00 ------------------------------------------------------------------------------------ 2028539- -1183 6139 44884.89 11.44 37.94 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 613 113660.59 15.98 69.33 1.73- 1.26 613 85269.52 21.27 59.05 1.26- 1.09 613 61580.33 18.94 67.70 1.09- 0.96 613 53980.31 14.72 33.61 0.96- 0.88 613 17318.14 7.09 43.72 0.88- 0.81 613 50327.72 14.18 36.70 0.80- 0.76 613 18363.99 5.73 18.11 0.76- 0.71 613 21182.54 6.93 16.97 0.71- 0.67 613 24179.39 7.95 28.55 0.67- 0.63 622 3592.58 1.77 6.11 ------------------------------------------------------------------------------------ 6.00- 0.63 6139 44884.89 11.44 37.94 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:45:57 2019 Sorting 6139 observations 43 unique observations with > 7.00 F2/sig(F2) 6139 observations in 6 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 Total number of frames 614 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 15 frame = 1 scale 6139 observations in 6 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 Total number of frames 42 1480 observations > 7.00 F2/sig(F2) 1480 observations in 6 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 Total number of frames 42 Removing 'redundancy=1' reflections Average redundancy: 26.9 (Out of 1480 removed 3 = 1477, unique = 55) 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 1477 observations in 6 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 Total number of frames 42 55 unique data precomputed (should be 55) 55 unique data with 1477 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 26.9 (Out of 1477 removed 0 = 1477, unique = 55) 55 unique data precomputed (should be 55) 55 unique data with 1477 observations RMS deviation of equivalent data = 0.31123 Rint = 0.25646 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24750, wR= 0.33855 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13177, wR= 0.18743, Acormin=0.460, Acormax=1.407, Acor_av=1.003 F test: Probability=1.000, F= 3.515 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12129, wR= 0.17435, Acormin=0.445, Acormax=1.465, Acor_av=0.969 F test: Probability=0.999, F= 1.178 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12544, wR= 0.17856, Acormin=0.540, Acormax=1.521, Acor_av=0.998 F test: Probability=0.000, F= 0.931 Trying model 4 (ne=4, no=1)... Results: Rint= 0.11016, wR= 0.16135, Acormin=0.432, Acormax=1.573, Acor_av=0.971 F test: Probability=1.000, F= 1.205 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09580, wR= 0.14679, Acormin=0.527, Acormax=1.807, Acor_av=1.012 F test: Probability=1.000, F= 1.316 Final absorption model (ne=4, no=3): Rint= 0.09580, Acormin=0.527, Acormax=1.807, Acor_av=1.012 Combined refinement in use Rint: 0.25823 There are 42 active scales (one needs to be fixed) Refinement control: frame scale #32 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 65 pars with 2145 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31123 Using Levenberg-Marquardt: 0.00010 New wR= 0.12205 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25646 with corrections 0.09087 Rint for all data: 0.25823 with corrections 0.09347 3 observations identified as outliers and rejected Cycle 2 wR= 0.11115 Using Levenberg-Marquardt: 0.00001 New wR= 0.08713 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25588 with corrections 0.06139 Rint for all data: 0.25823 with corrections 0.06769 0 observations identified as outliers and rejected Cycle 3 wR= 0.08713 Using Levenberg-Marquardt: 0.00000 New wR= 0.08348 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25588 with corrections 0.05768 Rint for all data: 0.25823 with corrections 0.06351 0 observations identified as outliers and rejected Cycle 4 wR= 0.08348 Using Levenberg-Marquardt: 0.00000 New wR= 0.08154 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25588 with corrections 0.05633 Rint for all data: 0.25823 with corrections 0.06212 0 observations identified as outliers and rejected Cycle 5 wR= 0.08154 Using Levenberg-Marquardt: 0.00000 New wR= 0.08053 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25588 with corrections 0.05544 Rint for all data: 0.25823 with corrections 0.06107 0 observations identified as outliers and rejected Final wR= 0.08053 Final frame scales: Min= 0.6601 Max= 1.2333 Final absorption correction factors: Amin= 0.3807 Amax= 1.5626 PROFFIT INFO: Inet (after scale3 abspack): min=-1102.5032 max=1262172.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=37.1939 max=24448.8047 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/104 6139 reflections read from tmp file 260 reflections are rejected (260 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 2 2 3 2 5 0 2 146 Initial Chi^2= 0.52411 Cycle 1, Chi^2= 1.01035 Current error model SIG(F2)^2 = 65.22*I_RAW + 10.46*I_BACK+(0.03473*)^2 Cycle 2, Chi^2= 1.01469 Current error model SIG(F2)^2 = 79.80*I_RAW + 6.95*I_BACK+(0.02802*)^2 Cycle 3, Chi^2= 1.00715 Current error model SIG(F2)^2 = 85.54*I_RAW + 5.80*I_BACK+(0.02655*)^2 Cycle 4, Chi^2= 1.00246 Current error model SIG(F2)^2 = 87.48*I_RAW + 5.45*I_BACK+(0.02627*)^2 Cycle 5, Chi^2= 1.00076 Current error model SIG(F2)^2 = 88.08*I_RAW + 5.35*I_BACK+(0.02620*)^2 Cycle 6, Chi^2= 1.00023 Current error model SIG(F2)^2 = 88.26*I_RAW + 5.32*I_BACK+(0.02618*)^2 Final Chi^2= 1.00023 Final error model SIG(F2)^2 = 88.26*I_RAW + 5.32*I_BACK+(0.02618*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1262172- 116388 613 377165.37 30.58 100.00 116194- 3443 613 29267.81 12.99 100.00 3434- 2003 613 2641.61 6.12 99.35 2000- 1140 613 1492.76 3.91 64.11 1138- 759 613 931.40 2.73 25.45 758- 514 613 634.56 2.37 15.33 514- 320 613 413.03 1.96 8.65 320- 148 613 235.91 1.46 3.10 148- 17 613 78.91 0.74 0.49 17- -1103 622 -129.50 -0.54 0.00 ------------------------------------------------------------------------------------ 1262172- -1103 6139 41212.49 6.22 41.59 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 613 105933.82 10.25 72.43 1.73- 1.26 613 78061.81 9.35 61.99 1.26- 1.09 613 56989.31 8.33 71.62 1.09- 0.96 613 48853.67 6.51 35.89 0.96- 0.88 613 15987.37 4.79 50.57 0.88- 0.81 613 46053.95 7.44 42.90 0.80- 0.76 613 16800.85 3.79 21.21 0.76- 0.71 613 18943.40 4.83 20.23 0.71- 0.67 613 21788.90 5.32 31.97 0.67- 0.63 622 3268.87 1.67 7.56 ------------------------------------------------------------------------------------ 6.00- 0.63 6139 41212.49 6.22 41.59 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.73 613 105933.82 10.25 72.43 6.00- 1.26 1226 91997.82 9.80 67.21 6.00- 1.09 1839 80328.31 9.31 68.68 6.00- 0.96 2452 72459.65 8.61 60.48 6.00- 0.88 3065 61165.20 7.85 58.50 6.00- 0.81 3678 58646.66 7.78 55.90 6.00- 0.76 4291 52668.68 7.21 50.94 6.00- 0.71 4904 48453.02 6.91 47.10 6.00- 0.67 5517 45490.34 6.74 45.42 6.00- 0.63 6139 41212.49 6.22 41.59 ------------------------------------------------------------------------------------ 6.00- 0.63 6139 41212.49 6.22 41.59 Scale applied to data: s=0.792284 (maximum obs:1262172.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.061; Rsigma 0.038: data 6139 -> merged 162 With outlier rejection... Rint 0.053; Rsigma 0.038: data 6122 -> merged 162 Rejected total: 17, method kkm 6, method Blessing 11 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626543, 6.009585 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.42 - 1.76 14 14 40.14 100.00 562 1.73 - 1.27 14 14 43.64 100.00 611 1.26 - 1.06 14 14 49.71 100.00 696 1.05 - 0.97 14 14 43.07 100.00 603 0.95 - 0.88 14 14 45.14 100.00 632 0.87 - 0.81 14 14 40.14 100.00 562 0.80 - 0.76 14 14 42.36 100.00 593 0.76 - 0.72 14 14 35.07 100.00 491 0.72 - 0.69 14 14 38.79 100.00 543 0.69 - 0.65 19 19 32.47 100.00 617 --------------------------------------------------------------- 10.42 - 0.65 145 145 40.76 100.00 5910 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:45:57 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.406731 10.415745 10.403771 89.9867 89.9811 90.0143 6117 Reflections read from file xs2212a.hkl 6084 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3052 0 4041 4033 6084 N (int>3sigma) = 0 0 0 0 1332 0 1774 1745 2514 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 34.3 32.2 32.9 Mean int/sigma = 0.0 0.0 0.0 0.0 3.9 0.0 6.6 6.4 6.4 Lattice type: F chosen Volume: 1127.70 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.356 7.359 7.360 119.99 119.96 90.02 Niggli form: a.a = 54.117 b.b = 54.152 c.c = 54.169 b.c = -27.069 a.c = -27.038 a.b = -0.015 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.087 CUBIC F-lattice R(int) = 0.048 [ 5853] Vol = 1127.7 Cell: 10.416 10.407 10.404 89.98 90.01 89.99 Volume: 1127.70 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.067 TETRAGONAL I-lattice R(int) = 0.047 [ 5467] Vol = 563.9 Cell: 7.361 7.363 10.404 90.00 89.98 89.95 Volume: 563.85 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.045 TETRAGONAL I-lattice R(int) = 0.047 [ 5467] Vol = 563.9 Cell: 7.356 7.359 10.416 90.00 89.98 90.02 Volume: 563.85 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.056 TETRAGONAL I-lattice R(int) = 0.047 [ 5467] Vol = 563.9 Cell: 7.363 7.361 10.404 90.02 90.00 90.05 Volume: 563.85 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.047 ORTHORHOMBIC F-lattice R(int) = 0.047 [ 5415] Vol = 1127.7 Cell: 10.404 10.407 10.416 89.99 90.01 89.98 Volume: 1127.70 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.074 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 5394] Vol = 563.9 Cell: 10.404 7.363 7.361 89.95 89.98 90.00 Volume: 563.85 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.027 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 5397] Vol = 563.9 Cell: 7.356 7.359 10.416 90.00 90.02 90.02 Volume: 563.85 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.043 MONOCLINIC I-lattice R(int) = 0.044 [ 4870] Vol = 563.9 Cell: 7.361 10.404 7.363 90.00 90.05 90.02 Volume: 563.85 Matrix:-0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.043 MONOCLINIC I-lattice R(int) = 0.045 [ 4868] Vol = 563.9 Cell: 7.360 10.407 7.362 90.00 90.07 89.98 Volume: 563.85 Matrix: 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.037 MONOCLINIC I-lattice R(int) = 0.044 [ 4870] Vol = 563.9 Cell: 7.363 10.404 7.361 90.02 90.05 90.00 Volume: 563.85 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.017 MONOCLINIC I-lattice R(int) = 0.044 [ 4858] Vol = 563.9 Cell: 7.356 7.359 10.416 90.00 90.02 89.98 Volume: 563.85 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.013 MONOCLINIC I-lattice R(int) = 0.044 [ 4871] Vol = 563.9 Cell: 7.356 10.416 7.359 90.00 90.02 89.98 Volume: 563.85 Matrix: 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.033 MONOCLINIC I-lattice R(int) = 0.044 [ 4871] Vol = 563.9 Cell: 7.356 10.416 7.359 90.00 90.02 90.02 Volume: 563.85 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 [ 3811] Vol = 281.9 Cell: 7.356 7.359 7.360 119.99 119.96 90.02 Volume: 281.93 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -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 3052 0 4045 4047 6084 N (int>3sigma) = 0 0 0 0 1332 0 1784 1771 2514 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 32.7 33.7 32.9 Mean int/sigma = 0.0 0.0 0.0 0.0 3.9 0.0 6.5 6.5 6.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.449 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 42 42 454 1199 N I>3s 2 2 2 636 0.0 0.0 0.0 2.0 0.8 0.8 0.2 5.0 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 0.048 5427 Fd-3m 1 1 227 C N N N N 37 2284 0.048 5489 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415745 10.406731 10.403771 89.9811 90.0133 89.9857 ZERR 5.00 0.001473 0.001328 0.001068 0.0095 0.0101 0.0109 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1135292- 89004 749 737 27 27.3 324633.22 28.60 0.050 0.065 74175- 1786 1161 1157 27 42.9 5057.15 8.18 0.087 0.092 1630- 758 1230 1229 27 45.5 1097.72 2.92 0.227 0.303 756- 316 1212 1212 27 44.9 488.33 2.02 0.367 0.524 309- 74 872 872 27 32.3 202.42 1.16 0.631 1.217 71- -178 915 915 27 33.9 12.33 0.20 0.961 4.384 ------------------------------------------------------------------------------------------- 1135292- -178 6139 6122 162 37.8 40384.61 6.17 0.053 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-1.27 1178 1172 27 43.4 93315.99 10.05 0.048 0.059 0.029 1.26-0.97 1239 1234 27 45.7 51017.87 7.24 0.048 0.063 0.035 0.97-0.81 1205 1203 27 44.6 31523.85 6.21 0.062 0.084 0.043 0.81-0.73 1063 1063 27 39.4 11062.04 3.16 0.065 0.086 0.064 0.73-0.67 920 918 27 34.0 25440.19 5.79 0.070 0.089 0.057 0.67-0.63 534 532 27 19.7 3526.20 1.74 0.119 0.090 0.135 ------------------------------------------------------------------------------------------------------ inf-0.63 6139 6122 162 37.8 40384.61 6.17 0.053 0.068 0.038 inf-0.65 5924 5909 144 41.0 41628.15 6.32 0.053 0.067 0.038 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-1.27 1172 27 27 100.0 43.4 93315.99 63.15 0.048 0.006 1.26-0.97 1234 27 27 100.0 45.7 51017.87 46.22 0.048 0.006 0.97-0.81 1203 27 27 100.0 44.6 31523.85 40.93 0.062 0.008 0.81-0.73 1063 27 27 100.0 39.4 11062.04 18.63 0.065 0.012 0.73-0.67 918 27 27 100.0 34.0 25440.19 34.53 0.070 0.010 0.67-0.63 532 27 27 100.0 19.7 3526.20 7.92 0.119 0.031 -------------------------------------------------------------------------------------------- inf-0.63 6122 162 162 100.0 37.8 40384.61 38.55 0.053 0.008 inf-0.65 5909 144 144 100.0 41.0 41628.15 39.72 0.053 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:52:03 2019) ID: 3668; threads 40; handles 811; mem 515164.00 (1204692.00)kB; time: 1w 5d 1h 2m 50s MEMORY INFO: Memory PF:225.0, Ph:551.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.1,peak PF: 700.2, WS: 471.1, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:227.0, Ph:552.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.9,peak PF: 700.2, WS: 472.9, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:52:03 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000013 0.000014 0.000014 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000013 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000014 ) 10.42433 ( 0.00206 ) 10.43788 ( 0.00196 ) 10.40727 ( 0.00215 ) 89.88512 ( 0.01613 ) 89.79539 ( 0.01640 ) 90.20497 ( 0.01572 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:52:03 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000013 0.000014 0.000014 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000013 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000014 ) M - matrix: 0.004646 0.000001 -0.000011 ( 0.000002 0.000001 0.000001 ) 0.000001 0.004641 -0.000001 ( 0.000001 0.000002 0.000001 ) -0.000011 -0.000001 0.004651 ( 0.000001 0.000001 0.000002 ) unit cell: 10.424(2) 10.438(2) 10.407(2) 89.885(16) 89.795(16) 90.205(16) V = 1132.4(4) unit cell: 10.4064(6) 10.4064(6) 10.4064(6) 90.0 90.0 90.0 V = 1126.93(12) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 218 peaks identified as outliers and rejected 218 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 218 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 218 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.60 | 22 | 0.998 ( 0.544) | 0.879 ( 0.218) | 1.641 ( 2.386) | 2.60- 1.76 | 22 | 0.823 ( 0.086) | 0.809 ( 0.143) | 0.780 ( 0.409) | 1.76- 1.57 | 22 | 0.861 ( 0.093) | 0.897 ( 0.150) | 0.733 ( 0.321) | 1.57- 1.35 | 22 | 0.917 ( 0.075) | 0.984 ( 0.122) | 1.028 ( 0.502) | 1.35- 1.16 | 22 | 0.956 ( 0.070) | 1.027 ( 0.132) | 1.031 ( 0.676) | 1.15- 1.00 | 22 | 0.917 ( 0.086) | 0.947 ( 0.167) | 0.994 ( 0.439) | 1.00- 0.88 | 22 | 0.964 ( 0.077) | 1.013 ( 0.129) | 1.167 ( 0.477) | 0.88- 0.79 | 22 | 0.981 ( 0.056) | 1.023 ( 0.138) | 1.203 ( 0.380) | 0.79- 0.69 | 22 | 0.977 ( 0.046) | 0.944 ( 0.101) | 1.277 ( 0.475) | 0.69- 0.63 | 20 | 0.946 ( 0.038) | 0.921 ( 0.084) | 1.348 ( 0.489) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 218 | 0.934 ( 0.193) | 0.945 ( 0.158) | 1.118 ( 0.917) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.87 | 25 | 0.945 ( 0.067) | 0.936 ( 0.094) | 1.074 ( 0.403) | 0.86- 0.73 | 25 | 0.958 ( 0.050) | 0.919 ( 0.091) | 1.335 ( 0.450) | 0.73- 0.63 | 29 | 0.929 ( 0.037) | 0.880 ( 0.095) | 1.340 ( 0.463) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 254 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.061 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.156) HKL list info: 1283 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 191 peaks identified as outliers and rejected 191 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 191 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 191 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.97 | 19 | 0.842 ( 0.116) | 0.844 ( 0.171) | 0.956 ( 0.449) | 2.63- 1.84 | 19 | 0.823 ( 0.110) | 0.841 ( 0.189) | 0.851 ( 0.503) | 1.83- 1.59 | 19 | 0.845 ( 0.105) | 0.839 ( 0.161) | 0.831 ( 0.357) | 1.59- 1.36 | 19 | 0.949 ( 0.088) | 0.994 ( 0.128) | 0.826 ( 0.266) | 1.36- 1.20 | 19 | 0.952 ( 0.104) | 0.977 ( 0.165) | 0.839 ( 0.328) | 1.17- 1.01 | 19 | 0.986 ( 0.080) | 1.005 ( 0.133) | 1.094 ( 0.438) | 1.01- 0.88 | 19 | 1.009 ( 0.084) | 1.029 ( 0.138) | 1.036 ( 0.361) | 0.88- 0.79 | 19 | 1.032 ( 0.057) | 1.041 ( 0.107) | 0.938 ( 0.316) | 0.79- 0.70 | 19 | 1.029 ( 0.055) | 0.987 ( 0.145) | 1.275 ( 0.529) | 0.70- 0.63 | 20 | 0.975 ( 0.053) | 0.882 ( 0.060) | 1.182 ( 0.417) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 191 | 0.944 ( 0.116) | 0.944 ( 0.163) | 0.984 ( 0.432) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 191 obs out of 191 (total:191,skipped:0) (100.00%) UB - matrix: 0.065810 0.015591 0.006263 ( 0.000023 0.000019 0.000022 ) -0.016403 0.064531 0.013131 ( 0.000023 0.000020 0.000022 ) -0.002751 -0.014148 0.066419 ( 0.000026 0.000022 0.000025 ) M - matrix: 0.004608 0.000006 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004607 0.000005 ( 0.000002 0.000003 0.000002 ) 0.000014 0.000005 0.004623 ( 0.000002 0.000002 0.000003 ) unit cell: 10.450(3) 10.450(3) 10.432(4) 90.07(3) 90.17(3) 90.08(3) V = 1139.1(6) OTKP changes: 191 1 1 1 OTKP changes: 191 1 1 1 No constraint UB - matrix: 0.066056 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016417 0.064704 0.013077 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066611 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066056 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016417 0.064704 0.013077 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066611 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) UB fit with 191 obs out of 191 (total:191,skipped:0) (100.00%) unit cell: 10.412(3) 10.418(3) 10.404(2) 89.85(2) 90.173(19) 90.09(2) V = 1128.5(5) unit cell: 10.4112(6) 10.4112(6) 10.4112(6) 90.0 90.0 90.0 V = 1128.49(12) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.025) HKL list info: 1278 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066056 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016417 0.064704 0.013077 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066611 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066056 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016417 0.064704 0.013077 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066611 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) UB fit with 191 obs out of 191 (total:191,skipped:0) (100.00%) unit cell: 10.412(3) 10.418(3) 10.404(2) 89.85(2) 90.173(19) 90.09(2) V = 1128.5(5) unit cell: 10.4112(6) 10.4112(6) 10.4112(6) 90.0 90.0 90.0 V = 1128.49(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 191 obs out of 191 (total:191,skipped:0) (100.00%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 191 peaks identified as outliers and rejected 191 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 191 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 191 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 3.00 | 19 | 0.846 ( 0.114) | 0.847 ( 0.168) | 0.873 ( 0.500) | 2.99- 2.00 | 19 | 0.802 ( 0.108) | 0.800 ( 0.186) | 0.843 ( 0.452) | 1.84- 1.64 | 19 | 0.841 ( 0.097) | 0.832 ( 0.150) | 0.879 ( 0.351) | 1.59- 1.36 | 19 | 0.936 ( 0.096) | 0.958 ( 0.162) | 0.847 ( 0.257) | 1.36- 1.20 | 19 | 0.949 ( 0.093) | 0.960 ( 0.151) | 0.779 ( 0.214) | 1.19- 1.01 | 19 | 1.019 ( 0.059) | 1.043 ( 0.127) | 1.050 ( 0.364) | 1.00- 0.88 | 19 | 1.011 ( 0.085) | 1.033 ( 0.121) | 1.040 ( 0.369) | 0.88- 0.78 | 19 | 1.027 ( 0.057) | 1.042 ( 0.117) | 0.971 ( 0.341) | 0.78- 0.69 | 19 | 1.036 ( 0.055) | 1.011 ( 0.164) | 1.296 ( 0.521) | 0.69- 0.63 | 20 | 0.970 ( 0.049) | 0.878 ( 0.054) | 1.110 ( 0.362) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 191 | 0.944 ( 0.117) | 0.940 ( 0.169) | 0.969 ( 0.412) | 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\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb PROFFITPEAK info: 91 peaks in the peak location table UB fit with 40 obs out of 57 (total:57,skipped:0) (70.18%) UB - matrix: 0.066061 0.015187 0.006486 ( 0.000308 0.000098 0.000090 ) -0.015888 0.064793 0.013313 ( 0.000150 0.000047 0.000044 ) -0.003040 -0.014343 0.066493 ( 0.000235 0.000074 0.000069 ) M - matrix: 0.004626 0.000017 0.000015 ( 0.000041 0.000013 0.000017 ) 0.000017 0.004635 0.000007 ( 0.000013 0.000007 0.000006 ) 0.000015 0.000007 0.004641 ( 0.000017 0.000006 0.000009 ) unit cell: 10.43(4) 10.419(11) 10.412(11) 90.09(9) 90.2(2) 90.22(17) V = 1131(5) UB fit with 40 obs out of 57 (total:57,skipped:0) (70.18%) UB - matrix: 0.066061 0.015187 0.006486 ( 0.000308 0.000098 0.000090 ) -0.015888 0.064793 0.013313 ( 0.000150 0.000047 0.000044 ) -0.003040 -0.014343 0.066493 ( 0.000235 0.000074 0.000069 ) M - matrix: 0.004626 0.000017 0.000015 ( 0.000041 0.000013 0.000017 ) 0.000017 0.004635 0.000007 ( 0.000013 0.000007 0.000006 ) 0.000015 0.000007 0.004641 ( 0.000017 0.000006 0.000009 ) unit cell: 10.43(4) 10.419(11) 10.412(11) 90.09(9) 90.2(2) 90.22(17) V = 1131(5) OTKP changes: 21 1 1 1 OTKP changes: 21 1 1 1 OTKP changes: 21 1 1 1 No constraint UB - matrix: 0.066072 0.015230 0.006085 ( 0.000198 0.000070 0.000062 ) -0.016135 0.064683 0.013492 ( 0.000115 0.000041 0.000036 ) -0.002400 -0.014403 0.066345 ( 0.000157 0.000056 0.000049 ) M - matrix: 0.004632 -0.000003 0.000025 ( 0.000026 0.000010 0.000011 ) -0.000003 0.004623 0.000010 ( 0.000010 0.000006 0.000005 ) 0.000025 0.000010 0.004621 ( 0.000011 0.000005 0.000007 ) Constraint UB - matrix: 0.066072 0.015230 0.006085 ( 0.000198 0.000070 0.000062 ) -0.016135 0.064683 0.013492 ( 0.000115 0.000041 0.000036 ) -0.002400 -0.014403 0.066345 ( 0.000157 0.000056 0.000049 ) M - matrix: 0.004621 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.004621 0.000000 ( 0.000000 0.000003 0.000000 ) 0.000000 0.000000 0.004621 ( 0.000000 0.000000 0.000003 ) UB fit with 53 obs out of 57 (total:57,skipped:0) (92.98%) unit cell: 10.42(3) 10.432(9) 10.435(8) 90.12(7) 90.31(14) 89.96(12) V = 1134(3) unit cell: 10.430(3) 10.430(3) 10.430(3) 90.0 90.0 90.0 V = 1134.5(6) UB fit with 53 obs out of 57 (total:57,skipped:0) (92.98%) UB - matrix: 0.066072 0.015230 0.006085 ( 0.000198 0.000070 0.000062 ) -0.016135 0.064683 0.013492 ( 0.000115 0.000041 0.000036 ) -0.002400 -0.014403 0.066345 ( 0.000157 0.000056 0.000049 ) M - matrix: 0.004632 -0.000003 0.000025 ( 0.000026 0.000010 0.000011 ) -0.000003 0.004623 0.000010 ( 0.000010 0.000006 0.000005 ) 0.000025 0.000010 0.004621 ( 0.000011 0.000005 0.000007 ) unit cell: 10.42(3) 10.432(9) 10.435(8) 90.12(7) 90.31(14) 89.96(12) V = 1134(3) OTKP changes: 22 1 1 1 OTKP changes: 22 1 1 1 OTKP changes: 22 1 1 1 No constraint UB - matrix: 0.066076 0.015231 0.006089 ( 0.000198 0.000070 0.000061 ) -0.016131 0.064677 0.013485 ( 0.000115 0.000041 0.000036 ) -0.002395 -0.014408 0.066338 ( 0.000156 0.000056 0.000049 ) M - matrix: 0.004632 -0.000002 0.000026 ( 0.000026 0.000010 0.000011 ) -0.000002 0.004623 0.000009 ( 0.000010 0.000006 0.000005 ) 0.000026 0.000009 0.004620 ( 0.000011 0.000005 0.000007 ) Constraint UB - matrix: 0.066076 0.015231 0.006089 ( 0.000198 0.000070 0.000061 ) -0.016131 0.064677 0.013485 ( 0.000115 0.000041 0.000036 ) -0.002395 -0.014408 0.066338 ( 0.000156 0.000056 0.000049 ) M - matrix: 0.004620 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.004620 0.000000 ( 0.000000 0.000003 0.000000 ) 0.000000 0.000000 0.004620 ( 0.000000 0.000000 0.000003 ) UB fit with 53 obs out of 57 (total:57,skipped:0) (92.98%) unit cell: 10.42(3) 10.432(9) 10.436(8) 90.11(7) 90.32(14) 89.97(12) V = 1135(3) unit cell: 10.430(3) 10.430(3) 10.430(3) 90.0 90.0 90.0 V = 1134.6(6) 57 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" Run 7 Omega scan: (-52.000 - -27.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 449 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 53 obs out of 57 (total:57,skipped:0) (92.98%) 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= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb 0 of 50 peaks identified as outliers and rejected 50 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 50 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 50 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.61 | 5 | 0.847 ( 0.116) | 0.832 ( 0.168) | 0.844 ( 0.402) | 2.40- 1.65 | 5 | 0.842 ( 0.100) | 0.825 ( 0.161) | 0.839 ( 0.482) | 1.65- 1.47 | 5 | 0.851 ( 0.144) | 0.816 ( 0.231) | 0.790 ( 0.193) | 1.47- 1.36 | 5 | 1.010 ( 0.054) | 1.042 ( 0.101) | 1.240 ( 0.493) | 1.36- 1.17 | 5 | 0.942 ( 0.131) | 0.923 ( 0.229) | 0.840 ( 0.061) | 1.17- 1.11 | 5 | 1.061 ( 0.206) | 0.912 ( 0.216) | 1.091 ( 0.635) | 1.00- 0.89 | 5 | 1.050 ( 0.058) | 1.097 ( 0.088) | 0.788 ( 0.142) | 0.89- 0.82 | 5 | 1.032 ( 0.109) | 1.140 ( 0.187) | 1.400 ( 0.467) | 0.82- 0.73 | 5 | 1.083 ( 0.043) | 1.128 ( 0.126) | 0.808 ( 0.073) | 0.70- 0.64 | 5 | 1.032 ( 0.053) | 1.012 ( 0.080) | 1.103 ( 0.495) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.64 | 50 | 0.975 ( 0.145) | 0.973 ( 0.207) | 0.974 ( 0.447) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) UB - matrix: 0.066053 0.015379 0.005987 ( 0.000112 0.000041 0.000034 ) -0.016238 0.064566 0.013359 ( 0.000110 0.000040 0.000034 ) -0.002632 -0.014495 0.066380 ( 0.000057 0.000021 0.000017 ) M - matrix: 0.004634 0.000006 0.000004 ( 0.000015 0.000008 0.000005 ) 0.000006 0.004615 -0.000008 ( 0.000008 0.000005 0.000003 ) 0.000004 -0.000008 0.004621 ( 0.000005 0.000003 0.000003 ) unit cell: 10.420(16) 10.441(8) 10.435(3) 89.91(4) 90.05(6) 90.07(10) V = 1135(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 No constraint UB - matrix: 0.065987 0.015315 0.005992 ( 0.000108 0.000039 0.000033 ) -0.016395 0.064674 0.013474 ( 0.000054 0.000020 0.000017 ) -0.002630 -0.014486 0.066394 ( 0.000053 0.000019 0.000016 ) M - matrix: 0.004630 -0.000012 -0.000000 ( 0.000014 0.000005 0.000004 ) -0.000012 0.004627 0.000001 ( 0.000005 0.000003 0.000002 ) -0.000000 0.000001 0.004626 ( 0.000004 0.000002 0.000002 ) Constraint UB - matrix: 0.065987 0.015315 0.005992 ( 0.000108 0.000039 0.000033 ) -0.016395 0.064674 0.013474 ( 0.000054 0.000020 0.000017 ) -0.002630 -0.014486 0.066394 ( 0.000053 0.000019 0.000016 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) unit cell: 10.424(15) 10.427(4) 10.429(3) 90.02(3) 90.00(5) 89.86(6) V = 1134(2) unit cell: 10.4269(13) 10.4269(13) 10.4269(13) 90.0 90.0 90.0 V = 1133.6(2) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-52.000 - -27.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 447 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb 0 of 50 peaks identified as outliers and rejected 50 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 50 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 50 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.60 | 5 | 0.848 ( 0.116) | 0.833 ( 0.168) | 1.065 ( 0.407) | 2.39- 1.65 | 5 | 0.835 ( 0.092) | 0.822 ( 0.168) | 0.636 ( 0.186) | 1.65- 1.46 | 5 | 0.860 ( 0.152) | 0.818 ( 0.232) | 1.069 ( 0.403) | 1.46- 1.36 | 5 | 1.027 ( 0.058) | 1.066 ( 0.112) | 1.136 ( 0.503) | 1.35- 1.16 | 5 | 0.927 ( 0.114) | 0.906 ( 0.195) | 0.969 ( 0.349) | 1.15- 1.00 | 5 | 0.989 ( 0.115) | 1.010 ( 0.232) | 0.728 ( 0.111) | 1.00- 0.88 | 5 | 1.031 ( 0.051) | 1.209 ( 0.243) | 0.747 ( 0.212) | 0.88- 0.82 | 5 | 1.052 ( 0.086) | 1.080 ( 0.082) | 1.172 ( 0.435) | 0.78- 0.70 | 5 | 1.067 ( 0.045) | 1.120 ( 0.128) | 1.079 ( 0.507) | 0.69- 0.63 | 5 | 1.021 ( 0.061) | 0.994 ( 0.084) | 0.940 ( 0.196) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.63 | 50 | 0.966 ( 0.128) | 0.986 ( 0.217) | 0.954 ( 0.400) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.2 | 145 | 0.992 ( 0.042) | 1.039 ( 0.071) | 1.123 ( 0.499) | 10.2-15.0 | 145 | 0.995 ( 0.048) | 1.052 ( 0.071) | 1.098 ( 0.503) | 15.0-19.3 | 145 | 0.995 ( 0.178) | 1.036 ( 0.098) | 1.107 ( 0.937) | 19.4-23.6 | 145 | 0.971 ( 0.067) | 1.010 ( 0.087) | 0.948 ( 0.416) | 23.7-27.7 | 145 | 0.972 ( 0.070) | 1.013 ( 0.115) | 0.966 ( 0.448) | 27.7-32.8 | 145 | 0.947 ( 0.085) | 0.962 ( 0.112) | 0.933 ( 0.439) | 32.9-36.5 | 145 | 0.914 ( 0.155) | 0.900 ( 0.150) | 1.051 ( 0.651) | 36.5-39.0 | 145 | 0.894 ( 0.108) | 0.887 ( 0.245) | 1.005 ( 0.469) | 39.0-42.0 | 145 | 0.896 ( 0.107) | 0.840 ( 0.144) | 1.028 ( 0.458) | 42.0-50.2 | 140 | 0.867 ( 0.126) | 0.794 ( 0.145) | 0.924 ( 0.416) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.2 | 1445 | 0.945 ( 0.116) | 0.954 ( 0.159) | 1.019 ( 0.550) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.14 e2 dimension: a=-0.0069 b=1.24 e3 dimension: a=0.0002 b=1.10 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 4496 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 14:52:23 2019 PROFFITMAIN - Started at Wed Aug 21 14:52:23 2019 OTKP changes: 1129 2 6 7 OTKP changes: 1129 2 6 7 OTKP changes: 1129 2 6 7 No constraint UB - matrix: 0.066149 0.015102 0.006696 ( 0.000013 0.000014 0.000013 ) -0.016213 0.064858 0.013206 ( 0.000012 0.000012 0.000012 ) -0.003632 -0.014434 0.066545 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004652 -0.000000 -0.000013 ( 0.000002 0.000001 0.000001 ) -0.000000 0.004643 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000013 -0.000003 0.004647 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066149 0.015102 0.006696 ( 0.000013 0.000014 0.000013 ) -0.016213 0.064858 0.013206 ( 0.000012 0.000012 0.000012 ) -0.003632 -0.014434 0.066545 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000001 ) UB fit with 1159 obs out of 1445 (total:1445,skipped:0) (80.21%) unit cell: 10.3998(19) 10.4096(19) 10.405(2) 89.965(16) 89.841(16) 89.998(15) V = 1126.4(4) unit cell: 10.4046(7) 10.4046(7) 10.4046(7) 90.0 90.0 90.0 V = 1126.37(12) *** 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 185 obs out of 218 (total:218,skipped:0) (84.86%) UB - matrix: 0.066501 0.011703 0.008961 ( 0.000033 0.000043 0.000036 ) -0.013687 0.065060 0.013250 ( 0.000031 0.000041 0.000034 ) -0.006054 -0.013932 0.065930 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.61(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 187 1 1 1 OTKP changes: 187 1 1 1 No constraint UB - matrix: 0.066497 0.011709 0.008954 ( 0.000032 0.000043 0.000035 ) -0.013711 0.065053 0.013254 ( 0.000032 0.000042 0.000035 ) -0.006056 -0.013930 0.065946 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000014 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004563 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000048 0.004605 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066497 0.011709 0.008954 ( 0.000032 0.000043 0.000035 ) -0.013711 0.065053 0.013254 ( 0.000032 0.000042 0.000035 ) -0.006056 -0.013930 0.065946 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000002 ) UB fit with 188 obs out of 218 (total:218,skipped:0) (86.24%) unit cell: 10.406(5) 10.501(6) 10.453(6) 90.61(5) 90.18(4) 89.64(4) V = 1142(1) unit cell: 10.4531(19) 10.4531(19) 10.4531(19) 90.0 90.0 90.0 V = 1142.2(3) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.138) HKL list info: 1310 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066497 0.011708 0.008954 ( 0.000032 0.000043 0.000035 ) -0.013711 0.065053 0.013254 ( 0.000032 0.000042 0.000035 ) -0.006056 -0.013930 0.065946 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000014 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004563 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000048 0.004605 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066497 0.011708 0.008954 ( 0.000032 0.000043 0.000035 ) -0.013711 0.065053 0.013254 ( 0.000032 0.000042 0.000035 ) -0.006056 -0.013930 0.065946 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000002 ) UB fit with 188 obs out of 218 (total:218,skipped:0) (86.24%) unit cell: 10.406(5) 10.501(6) 10.453(6) 90.61(5) 90.18(4) 89.64(4) V = 1142(1) unit cell: 10.4531(19) 10.4531(19) 10.4531(19) 90.0 90.0 90.0 V = 1142.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 202 obs out of 218 (total:218,skipped:0) (92.66%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068142 -0.000274 0.000126 ( 0.000028 0.000036 0.000029 ) -0.000077 0.067601 0.000625 ( 0.000032 0.000041 0.000033 ) -0.000032 -0.000064 0.067958 ( 0.000023 0.000030 0.000024 ) M - matrix: 0.004643 -0.000024 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000024 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000038 0.004619 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068142 -0.000274 0.000126 ( 0.000028 0.000036 0.000029 ) -0.000077 0.067601 0.000625 ( 0.000032 0.000041 0.000033 ) -0.000032 -0.000064 0.067958 ( 0.000023 0.000030 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 204 obs out of 218 (total:218,skipped:0) (93.58%) unit cell: 10.409(4) 10.493(6) 10.437(4) 90.47(4) 90.08(3) 89.70(4) V = 1139.9(9) unit cell: 10.4463(13) 10.4463(13) 10.4463(13) 90.0 90.0 90.0 V = 1139.9(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.066336 0.014186 0.006779 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064704 0.012861 ( 0.000017 0.000022 0.000023 ) -0.004076 -0.014197 0.066901 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.393(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4047(5) 10.4047(5) 10.4047(5) 90.0 90.0 90.0 V = 1126.40(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065883 0.015205 0.006808 ( 0.000019 0.000013 0.000019 ) -0.016068 0.064785 0.013231 ( 0.000017 0.000012 0.000016 ) -0.003637 -0.014505 0.066499 ( 0.000021 0.000015 0.000021 ) M - matrix: 0.004612 0.000014 -0.000006 ( 0.000003 0.000001 0.000002 ) 0.000014 0.004639 -0.000004 ( 0.000001 0.000002 0.000002 ) -0.000006 -0.000004 0.004644 ( 0.000002 0.000002 0.000003 ) unit cell: 10.444(3) 10.414(2) 10.409(3) 89.952(19) 89.93(2) 90.168(19) V = 1132.2(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065935 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064847 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066576 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065935 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064847 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066576 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4060(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1129.0(5) unit cell: 10.4126(5) 10.4126(5) 10.4126(5) 90.0 90.0 90.0 V = 1128.96(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.032) HKL list info: 1274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065935 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064847 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066576 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065935 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064847 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066576 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4060(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1129.0(5) unit cell: 10.4126(5) 10.4126(5) 10.4126(5) 90.0 90.0 90.0 V = 1128.96(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065935 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064847 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066576 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065935 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064847 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066576 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4060(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1129.0(5) unit cell: 10.4126(5) 10.4126(5) 10.4126(5) 90.0 90.0 90.0 V = 1128.96(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066117 0.015252 0.006582 ( 0.000015 0.000020 0.000017 ) -0.016341 0.064736 0.012926 ( 0.000012 0.000016 0.000013 ) -0.003352 -0.014201 0.066518 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004650 -0.000002 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000002 0.004625 -0.000007 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000007 0.004635 ( 0.000001 0.000001 0.000002 ) unit cell: 10.402(2) 10.430(2) 10.4185(19) 89.907(16) 90.012(17) 89.977(19) V = 1130.3(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066154 0.015270 0.006525 ( 0.000013 0.000018 0.000015 ) -0.016368 0.064790 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003344 -0.014170 0.066612 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004655 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004632 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066154 0.015270 0.006525 ( 0.000013 0.000018 0.000015 ) -0.016368 0.064790 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003344 -0.014170 0.066612 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.396(2) 10.422(2) 10.4042(18) 89.945(16) 89.960(15) 89.965(18) V = 1127.3(4) unit cell: 10.4073(5) 10.4073(5) 10.4073(5) 90.0 90.0 90.0 V = 1127.25(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.032) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066154 0.015270 0.006525 ( 0.000013 0.000018 0.000015 ) -0.016368 0.064790 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003344 -0.014170 0.066612 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004655 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004632 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066154 0.015270 0.006525 ( 0.000013 0.000018 0.000015 ) -0.016368 0.064790 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003344 -0.014170 0.066612 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.396(2) 10.422(2) 10.4042(18) 89.945(16) 89.960(15) 89.965(18) V = 1127.3(4) unit cell: 10.4073(5) 10.4073(5) 10.4073(5) 90.0 90.0 90.0 V = 1127.25(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068215 -0.000038 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068072 -0.000054 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068176 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004653 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004634 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068215 -0.000038 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068072 -0.000054 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068176 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.3980(16) 10.420(3) 10.4039(15) 89.964(16) 89.976(13) 89.968(17) V = 1127.2(4) unit cell: 10.4073(5) 10.4073(5) 10.4073(5) 90.0 90.0 90.0 V = 1127.22(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 260 obs out of 271 (total:271,skipped:0) (95.94%) UB - matrix: 0.065971 0.015326 0.006329 ( 0.000016 0.000012 0.000013 ) -0.016393 0.064803 0.013404 ( 0.000020 0.000015 0.000015 ) -0.002994 -0.014554 0.066487 ( 0.000023 0.000017 0.000018 ) M - matrix: 0.004630 -0.000008 -0.000001 ( 0.000002 0.000002 0.000002 ) -0.000008 0.004646 -0.000002 ( 0.000002 0.000002 0.000002 ) -0.000001 -0.000002 0.004640 ( 0.000002 0.000002 0.000002 ) unit cell: 10.424(2) 10.406(2) 10.413(3) 89.97(2) 89.98(2) 89.90(2) V = 1129.5(5) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.066050 0.015388 0.006334 ( 0.000016 0.000012 0.000013 ) -0.016396 0.064848 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002877 -0.014635 0.066564 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004656 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004650 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066050 0.015388 0.006334 ( 0.000016 0.000012 0.000013 ) -0.016396 0.064848 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002877 -0.014635 0.066564 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.413(2) 10.395(2) 10.4018(18) 89.887(15) 90.092(17) 89.941(18) V = 1125.9(4) unit cell: 10.4032(5) 10.4032(5) 10.4032(5) 90.0 90.0 90.0 V = 1125.92(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.032) HKL list info: 1297 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066050 0.015388 0.006334 ( 0.000016 0.000012 0.000013 ) -0.016396 0.064848 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002877 -0.014635 0.066564 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004656 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004650 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066050 0.015388 0.006334 ( 0.000016 0.000012 0.000013 ) -0.016396 0.064848 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002877 -0.014635 0.066564 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.413(2) 10.395(2) 10.4018(18) 89.887(15) 90.092(17) 89.941(18) V = 1125.9(4) unit cell: 10.4032(5) 10.4032(5) 10.4032(5) 90.0 90.0 90.0 V = 1125.92(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068121 -0.000095 0.000071 ( 0.000017 0.000013 0.000014 ) 0.000059 0.068206 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068183 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004652 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068121 -0.000095 0.000071 ( 0.000017 0.000013 0.000014 ) 0.000059 0.068206 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068183 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.412(3) 10.3994(16) 10.4029(18) 89.931(13) 90.044(17) 89.971(16) V = 1126.5(4) unit cell: 10.4049(5) 10.4049(5) 10.4049(5) 90.0 90.0 90.0 V = 1126.46(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 191 obs out of 191 (total:191,skipped:0) (100.00%) UB - matrix: 0.066050 0.015580 0.006343 ( 0.000018 0.000015 0.000018 ) -0.016417 0.064706 0.013083 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014361 0.066612 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004640 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004636 -0.000011 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000011 0.004649 ( 0.000002 0.000002 0.000002 ) unit cell: 10.413(3) 10.418(3) 10.403(2) 89.86(2) 90.166(19) 90.10(2) V = 1128.5(5) OTKP changes: 191 1 1 1 OTKP changes: 191 1 1 1 OTKP changes: 191 1 1 1 OTKP changes: 191 1 1 1 OTKP changes: 191 1 1 1 OTKP changes: 191 1 1 1 Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.025) HKL list info: 1264 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066050 0.015580 0.006343 ( 0.000018 0.000015 0.000018 ) -0.016417 0.064706 0.013083 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014361 0.066612 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004640 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004636 -0.000011 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000011 0.004649 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066050 0.015580 0.006343 ( 0.000018 0.000015 0.000018 ) -0.016417 0.064706 0.013083 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014361 0.066612 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) UB fit with 191 obs out of 191 (total:191,skipped:0) (100.00%) unit cell: 10.413(3) 10.418(3) 10.403(2) 89.86(2) 90.166(19) 90.10(2) V = 1128.5(5) unit cell: 10.4111(7) 10.4111(7) 10.4111(7) 90.0 90.0 90.0 V = 1128.48(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 191 obs out of 191 (total:191,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: 0.068147 0.000080 0.000193 ( 0.000019 0.000016 0.000019 ) -0.000013 0.068092 -0.000152 ( 0.000021 0.000017 0.000020 ) -0.000002 -0.000000 0.068176 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004644 0.000005 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000005 0.004637 -0.000010 ( 0.000002 0.000002 0.000002 ) 0.000013 -0.000010 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.068147 0.000080 0.000193 ( 0.000019 0.000016 0.000019 ) -0.000013 0.068092 -0.000152 ( 0.000021 0.000017 0.000020 ) -0.000002 -0.000000 0.068176 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000001 ) UB fit with 191 obs out of 191 (total:191,skipped:0) (100.00%) unit cell: 10.408(3) 10.417(3) 10.4039(18) 89.872(19) 90.160(19) 90.06(2) V = 1128.0(5) unit cell: 10.4097(6) 10.4097(6) 10.4097(6) 90.0 90.0 90.0 V = 1128.01(12) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.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= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 43 obs out of 50 (total:50,skipped:0) (86.00%) UB - matrix: 0.065747 0.015173 0.006311 ( 0.000204 0.000071 0.000067 ) -0.016246 0.064699 0.013354 ( 0.000088 0.000031 0.000029 ) -0.002758 -0.014393 0.066493 ( 0.000127 0.000044 0.000042 ) M - matrix: 0.004594 -0.000014 0.000015 ( 0.000027 0.000008 0.000010 ) -0.000014 0.004623 0.000003 ( 0.000008 0.000005 0.000004 ) 0.000015 0.000003 0.004640 ( 0.000010 0.000004 0.000006 ) unit cell: 10.46(3) 10.432(7) 10.413(7) 90.03(6) 90.18(12) 89.83(11) V = 1137(3) OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 OTKP changes: 49 1 1 1 No constraint UB - matrix: 0.066289 0.015345 0.005979 ( 0.000110 0.000040 0.000036 ) -0.016398 0.064771 0.013502 ( 0.000056 0.000020 0.000018 ) -0.002586 -0.014516 0.066504 ( 0.000056 0.000020 0.000018 ) M - matrix: 0.004670 -0.000007 0.000003 ( 0.000015 0.000005 0.000005 ) -0.000007 0.004641 0.000001 ( 0.000005 0.000003 0.000002 ) 0.000003 0.000001 0.004641 ( 0.000005 0.000002 0.000003 ) Constraint UB - matrix: 0.066289 0.015345 0.005979 ( 0.000110 0.000040 0.000036 ) -0.016398 0.064771 0.013502 ( 0.000056 0.000020 0.000018 ) -0.002586 -0.014516 0.066504 ( 0.000056 0.000020 0.000018 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) unit cell: 10.380(16) 10.411(4) 10.412(3) 90.01(3) 90.04(5) 89.91(6) V = 1125(2) unit cell: 10.4009(15) 10.4009(15) 10.4009(15) 90.0 90.0 90.0 V = 1125.2(3) Run 7 Omega scan: (-52.000 - -27.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.032) HKL list info: 428 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: 0.066289 0.015345 0.005979 ( 0.000110 0.000040 0.000036 ) -0.016398 0.064771 0.013502 ( 0.000056 0.000020 0.000018 ) -0.002586 -0.014516 0.066504 ( 0.000056 0.000020 0.000018 ) M - matrix: 0.004670 -0.000007 0.000003 ( 0.000015 0.000005 0.000005 ) -0.000007 0.004641 0.000001 ( 0.000005 0.000003 0.000002 ) 0.000003 0.000001 0.004641 ( 0.000005 0.000002 0.000003 ) Constraint UB - matrix: 0.066289 0.015345 0.005979 ( 0.000110 0.000040 0.000036 ) -0.016398 0.064771 0.013502 ( 0.000056 0.000020 0.000018 ) -0.002586 -0.014516 0.066504 ( 0.000056 0.000020 0.000018 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 50 obs out of 50 (total:50,skipped:0) (100.00%) unit cell: 10.380(16) 10.411(4) 10.412(3) 90.01(3) 90.04(5) 89.91(6) V = 1125(2) unit cell: 10.4009(15) 10.4009(15) 10.4009(15) 90.0 90.0 90.0 V = 1125.2(3) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068161 0.000013 -0.000045 ( 0.000009 0.000009 0.000009 ) -0.000004 0.068099 -0.000003 ( 0.000009 0.000009 0.000009 ) 0.000028 -0.000019 0.068177 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004646 0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.004637 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000002 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068161 0.000013 -0.000045 ( 0.000009 0.000009 0.000009 ) -0.000004 0.068099 -0.000003 ( 0.000009 0.000009 0.000009 ) 0.000028 -0.000019 0.068177 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 1420 obs out of 1445 (total:1445,skipped:0) (98.27%) unit cell: 10.4062(13) 10.4158(14) 10.4038(10) 89.981(10) 89.986(9) 90.008(11) V = 1127.7(2) unit cell: 10.4086(3) 10.4086(3) 10.4086(3) 90.0 90.0 90.0 V = 1127.66(6) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 167 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_7.rrpprof 6354 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:52:33 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.138) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.032) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.032) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.032) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.025) Run 7 Omega scan: (-52.000 - -27.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.032) PROFFIT INFO: signal sum: min=-765.0000 max=7910405.0000 PROFFIT INFO: signal sum lp corr: min=-739.5427 max=1266439.5035 PROFFIT INFO: background sum: min=-86.0000 max=8197.0000 PROFFIT INFO: background sum sig2: min=414.0000 max=5764.0000 PROFFIT INFO: num of signal pixels: min=41 max=506 PROFFIT INFO: Inet: min=-1183.2683 max=2026303.2500 PROFFIT INFO: sig(Inet): min=51.9829 max=30723.3379 PROFFIT INFO: Inet/sig(Inet): min=-2.09 max=276.14 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 551 2198 3314 3940 4249 4935 5361 5625 6020 6286 6354 Percent 8.7 34.6 52.2 62.0 66.9 77.7 84.4 88.5 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 6354 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 6354 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2026303- 130954 635 412522.92 77.68 100.00 129797- 4045 635 29117.79 19.51 100.00 4043- 2067 635 2873.55 7.05 97.01 2063- 1231 635 1588.05 3.96 52.76 1230- 812 635 1003.76 2.33 16.22 811- 540 635 668.52 1.73 8.35 539- 336 635 433.16 1.21 5.04 336- 155 635 243.08 0.70 0.79 155- 19 635 82.79 0.30 0.00 19- -1183 639 -136.29 -0.27 0.00 ------------------------------------------------------------------------------------ 2026303- -1183 6354 44811.42 11.41 37.99 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 635 112315.56 15.81 68.82 1.64- 1.26 635 85270.76 21.24 59.53 1.26- 1.06 635 62271.72 19.13 68.98 1.06- 0.96 635 52715.28 14.30 32.44 0.96- 0.88 635 19976.75 7.74 44.57 0.88- 0.80 635 48289.93 13.57 35.75 0.80- 0.76 635 18317.31 5.74 19.06 0.76- 0.71 635 21006.07 6.84 16.06 0.71- 0.67 635 24513.89 7.99 28.50 0.67- 0.63 639 3695.93 1.81 6.42 ------------------------------------------------------------------------------------ 6.00- 0.63 6354 44811.42 11.41 37.99 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:52:33 2019 Sorting 6354 observations 53 unique observations with > 7.00 F2/sig(F2) 6354 observations in 7 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 24 639 Total number of frames 639 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 13 frame = 1 scale 6354 observations in 7 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 1 50 Total number of frames 50 1533 observations > 7.00 F2/sig(F2) 1533 observations in 7 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 1 50 Total number of frames 50 Removing 'redundancy=1' reflections Average redundancy: 22.8 (Out of 1533 removed 8 = 1525, unique = 67) 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 1525 observations in 7 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 1 50 Total number of frames 50 67 unique data precomputed (should be 67) 67 unique data with 1525 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.8 (Out of 1525 removed 0 = 1525, unique = 67) 67 unique data precomputed (should be 67) 67 unique data with 1525 observations RMS deviation of equivalent data = 0.30881 Rint = 0.25207 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24321, wR= 0.33249 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13271, wR= 0.18573, Acormin=0.472, Acormax=1.420, Acor_av=1.004 F test: Probability=1.000, F= 3.347 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12502, wR= 0.17628, Acormin=0.472, Acormax=1.466, Acor_av=0.980 F test: Probability=0.987, F= 1.125 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12507, wR= 0.17627, Acormin=0.534, Acormax=1.537, Acor_av=1.005 F test: Probability=0.000, F= 0.995 Trying model 4 (ne=4, no=1)... Results: Rint= 0.11437, wR= 0.16415, Acormin=0.463, Acormax=1.569, Acor_av=0.985 F test: Probability=0.999, F= 1.187 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09917, wR= 0.14892, Acormin=0.534, Acormax=1.792, Acor_av=1.031 F test: Probability=1.000, F= 1.324 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12067, wR= 0.17027, Acormin=0.421, Acormax=1.600, Acor_av=0.987 F test: Probability=0.000, F= 0.674 Trying model 7 (ne=6, no=1)... Results: Rint= 0.11126, wR= 0.16068, Acormin=0.449, Acormax=1.594, Acor_av=0.979 F test: Probability=0.000, F= 0.791 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09713, wR= 0.14663, Acormin=0.529, Acormax=1.807, Acor_av=1.022 F test: Probability=0.729, F= 1.033 Trying model 9 (ne=6, no=5)... Results: Rint= 0.14192, wR= 0.18690, Acormin=0.092, Acormax=1.057, Acor_av=0.544 F test: Probability=0.000, F= 0.480 Final absorption model (ne=4, no=3): Rint= 0.09917, Acormin=0.534, Acormax=1.792, Acor_av=1.031 Combined refinement in use Rint: 0.25388 There are 50 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 73 pars with 2701 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30881 Using Levenberg-Marquardt: 0.00010 New wR= 0.11699 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25207 with corrections 0.09104 Rint for all data: 0.25388 with corrections 0.09366 3 observations identified as outliers and rejected Cycle 2 wR= 0.10585 Using Levenberg-Marquardt: 0.00001 New wR= 0.08923 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25181 with corrections 0.05958 Rint for all data: 0.25388 with corrections 0.06492 1 observations identified as outliers and rejected Cycle 3 wR= 0.08764 Using Levenberg-Marquardt: 0.00000 New wR= 0.08549 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25174 with corrections 0.05919 Rint for all data: 0.25388 with corrections 0.06543 0 observations identified as outliers and rejected Cycle 4 wR= 0.08549 Using Levenberg-Marquardt: 0.00000 New wR= 0.08510 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25174 with corrections 0.05879 Rint for all data: 0.25388 with corrections 0.06504 0 observations identified as outliers and rejected Cycle 5 wR= 0.08510 Using Levenberg-Marquardt: 0.00000 New wR= 0.08467 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25174 with corrections 0.05866 Rint for all data: 0.25388 with corrections 0.06491 0 observations identified as outliers and rejected Final wR= 0.08467 Final frame scales: Min= 0.7417 Max= 1.3325 Final absorption correction factors: Amin= 0.3055 Amax= 1.5518 PROFFIT INFO: Inet (after scale3 abspack): min=-1107.9344 max=1314988.6250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.6400 max=24288.5645 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/104 6354 reflections read from tmp file 278 reflections are rejected (277 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 6 4 5 3 5 3 3 210 Initial Chi^2= 0.52787 Cycle 1, Chi^2= 1.01588 Current error model SIG(F2)^2 = 64.07*I_RAW + 10.35*I_BACK+(0.03693*)^2 Cycle 2, Chi^2= 1.01640 Current error model SIG(F2)^2 = 79.27*I_RAW + 6.98*I_BACK+(0.02862*)^2 Cycle 3, Chi^2= 1.00840 Current error model SIG(F2)^2 = 85.71*I_RAW + 5.80*I_BACK+(0.02640*)^2 Cycle 4, Chi^2= 1.00292 Current error model SIG(F2)^2 = 87.97*I_RAW + 5.44*I_BACK+(0.02591*)^2 Cycle 5, Chi^2= 1.00086 Current error model SIG(F2)^2 = 88.65*I_RAW + 5.34*I_BACK+(0.02580*)^2 Cycle 6, Chi^2= 1.00024 Current error model SIG(F2)^2 = 88.84*I_RAW + 5.31*I_BACK+(0.02577*)^2 Final Chi^2= 1.00024 Final error model SIG(F2)^2 = 88.84*I_RAW + 5.31*I_BACK+(0.02577*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1314989- 116402 635 378184.66 30.86 100.00 115969- 3449 635 28895.64 12.89 100.00 3431- 2010 635 2655.99 6.08 99.21 2002- 1145 635 1497.83 3.90 63.62 1144- 765 635 938.58 2.73 25.67 765- 514 635 637.06 2.36 14.80 514- 324 635 411.36 1.95 8.35 324- 150 635 237.44 1.45 3.31 150- 19 635 81.27 0.75 0.47 19- -1108 639 -134.31 -0.56 0.00 ------------------------------------------------------------------------------------ 1314989- -1108 6354 41314.44 6.24 41.52 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 635 105309.04 10.19 71.97 1.64- 1.26 635 78686.05 9.39 62.05 1.26- 1.06 635 58344.42 8.50 72.76 1.06- 0.96 635 47461.84 6.37 34.65 0.96- 0.88 635 18072.62 5.06 51.81 0.88- 0.80 635 44405.46 7.23 41.57 0.80- 0.76 635 16860.96 3.82 21.73 0.76- 0.71 635 18800.99 4.77 19.37 0.71- 0.67 635 21990.47 5.34 31.81 0.67- 0.63 639 3451.09 1.72 7.67 ------------------------------------------------------------------------------------ 6.00- 0.63 6354 41314.44 6.24 41.52 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 635 105309.04 10.19 71.97 6.00- 1.26 1270 91997.55 9.79 67.01 6.00- 1.06 1905 80779.84 9.36 68.92 6.00- 0.96 2540 72450.34 8.61 60.35 6.00- 0.88 3175 61574.79 7.90 58.65 6.00- 0.80 3810 58713.24 7.79 55.80 6.00- 0.76 4445 52734.34 7.22 50.93 6.00- 0.71 5080 48492.67 6.92 46.99 6.00- 0.67 5715 45547.98 6.74 45.30 6.00- 0.63 6354 41314.44 6.24 41.52 ------------------------------------------------------------------------------------ 6.00- 0.63 6354 41314.44 6.24 41.52 Scale applied to data: s=0.760462 (maximum obs:1314988.625,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.065; Rsigma 0.037: data 6354 -> merged 240 With outlier rejection... Rint 0.056; Rsigma 0.038: data 6334 -> merged 240 Rejected total: 20, method kkm 8, method Blessing 12 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626524, 6.009405 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.41 - 1.59 21 21 34.48 100.00 724 1.57 - 1.20 21 21 35.95 100.00 755 1.19 - 1.02 21 21 33.81 100.00 710 1.02 - 0.91 21 21 32.38 100.00 680 0.91 - 0.84 21 21 28.76 100.00 604 0.84 - 0.78 21 21 28.29 100.00 594 0.78 - 0.74 21 21 26.71 100.00 561 0.74 - 0.71 21 21 22.57 100.00 474 0.71 - 0.68 21 21 25.00 100.00 525 0.68 - 0.65 23 23 21.17 100.00 487 --------------------------------------------------------------- 10.41 - 0.65 212 212 28.84 100.00 6114 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:52:34 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.406228 10.415771 10.403789 89.9813 89.9855 90.0082 6334 Reflections read from file xs2212a.hkl 6297 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.21 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3161 0 4181 4170 6297 N (int>3sigma) = 0 0 0 0 1393 0 1843 1813 2619 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.0 30.3 30.8 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.2 6.2 Lattice type: F chosen Volume: 1127.66 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.357 7.358 7.360 119.98 119.96 90.01 Niggli form: a.a = 54.118 b.b = 54.146 c.c = 54.164 b.c = -27.062 a.c = -27.040 a.b = -0.013 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.086 CUBIC F-lattice R(int) = 0.056 [ 6066] Vol = 1127.7 Cell: 10.416 10.406 10.404 89.99 90.02 89.99 Volume: 1127.66 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.055 TETRAGONAL I-lattice R(int) = 0.055 [ 5680] Vol = 563.8 Cell: 7.361 7.362 10.404 90.00 89.98 89.95 Volume: 563.83 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.036 TETRAGONAL I-lattice R(int) = 0.055 [ 5681] Vol = 563.8 Cell: 7.357 7.358 10.416 89.99 89.98 90.01 Volume: 563.83 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.067 TETRAGONAL I-lattice R(int) = 0.055 [ 5680] Vol = 563.8 Cell: 7.362 7.361 10.404 90.02 90.00 90.05 Volume: 563.83 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.032 ORTHORHOMBIC F-lattice R(int) = 0.054 [ 5627] Vol = 1127.7 Cell: 10.404 10.406 10.416 89.99 90.02 89.99 Volume: 1127.66 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.067 ORTHORHOMBIC I-lattice R(int) = 0.054 [ 5607] Vol = 563.8 Cell: 10.404 7.362 7.361 89.95 89.98 90.00 Volume: 563.83 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.026 ORTHORHOMBIC I-lattice R(int) = 0.053 [ 5607] Vol = 563.8 Cell: 7.357 7.358 10.416 90.01 90.02 90.01 Volume: 563.83 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.037 MONOCLINIC I-lattice R(int) = 0.052 [ 5080] Vol = 563.8 Cell: 7.361 10.404 7.362 90.00 90.05 90.02 Volume: 563.83 Matrix:-0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.032 MONOCLINIC I-lattice R(int) = 0.052 [ 5081] Vol = 563.8 Cell: 7.360 10.406 7.362 90.00 90.07 89.98 Volume: 563.83 Matrix: 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.030 MONOCLINIC I-lattice R(int) = 0.052 [ 5080] Vol = 563.8 Cell: 7.362 10.404 7.361 90.02 90.05 90.00 Volume: 563.83 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.023 MONOCLINIC I-lattice R(int) = 0.052 [ 5059] Vol = 563.8 Cell: 7.358 7.357 10.416 89.98 90.01 89.99 Volume: 563.83 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.017 MONOCLINIC I-lattice R(int) = 0.051 [ 5068] Vol = 563.8 Cell: 7.357 7.358 10.416 89.99 90.02 89.99 Volume: 563.83 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.014 MONOCLINIC I-lattice R(int) = 0.051 [ 5081] Vol = 563.8 Cell: 7.357 10.416 7.358 89.99 90.01 89.98 Volume: 563.83 Matrix: 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.040 MONOCLINIC I-lattice R(int) = 0.051 [ 5081] Vol = 563.8 Cell: 7.357 10.416 7.358 90.01 90.01 90.02 Volume: 563.83 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) = 0.047 [ 4020] Vol = 281.9 Cell: 7.357 7.358 7.360 119.98 119.96 90.01 Volume: 281.91 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -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 3161 0 4188 4189 6297 N (int>3sigma) = 0 0 0 0 1393 0 1855 1847 2619 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 30.4 31.6 30.8 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.3 6.2 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.424 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 45 45 474 1236 N I>3s 2 2 2 662 0.0 0.0 -0.0 1.9 0.8 0.8 0.2 5.0 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 0.055 5620 Fd-3m 1 1 227 C N N N N 37 2284 0.056 5682 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415771 10.406228 10.403789 89.9855 90.0187 89.9918 ZERR 5.00 0.001398 0.001328 0.001033 0.0093 0.0096 0.0106 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1132461- 124444 631 619 26 23.8 375803.27 30.76 0.051 0.069 106634- 3117 717 713 26 27.4 26536.27 12.12 0.072 0.083 2992- 1385 924 920 26 35.4 2200.70 5.50 0.133 0.187 1352- 821 804 804 26 30.9 1036.10 2.74 0.238 0.307 819- 492 775 775 26 29.8 637.02 2.29 0.305 0.411 488- 311 758 758 26 29.2 384.08 1.76 0.434 0.576 294- 140 582 582 26 22.4 222.98 1.29 0.588 1.058 139- 31 581 581 26 22.3 78.40 0.57 0.868 2.589 26- -188 582 582 32 18.2 -27.73 -0.05 0.996 4.377 ------------------------------------------------------------------------------------------- 1132461- -188 6354 6334 240 26.4 40313.27 6.17 0.056 0.075 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-1.44 934 928 26 35.7 112392.62 11.10 0.049 0.065 0.029 1.39-1.09 968 965 26 37.1 44048.08 7.34 0.051 0.072 0.034 1.06-0.94 810 807 26 31.0 38056.29 5.61 0.050 0.068 0.036 0.92-0.84 772 771 26 29.7 41367.70 7.44 0.062 0.085 0.041 0.84-0.78 750 749 26 28.8 24146.12 4.96 0.065 0.086 0.048 0.78-0.73 666 666 27 24.7 13133.80 3.80 0.079 0.101 0.064 0.72-0.69 643 642 26 24.7 14029.73 3.85 0.078 0.087 0.068 0.68-0.66 581 579 27 21.4 14339.38 3.81 0.080 0.109 0.068 0.65-0.63 230 227 30 7.6 7882.94 2.38 0.083 0.082 0.087 ------------------------------------------------------------------------------------------------------ inf-0.63 6354 6334 240 26.4 40313.27 6.17 0.056 0.075 0.038 inf-0.65 6129 6112 211 29.0 41559.19 6.33 0.055 0.074 0.037 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-1.44 928 26 26 100.0 35.7 112392.62 66.52 0.049 0.006 1.39-1.09 965 26 26 100.0 37.1 44048.08 40.65 0.051 0.007 1.06-0.94 807 26 26 100.0 31.0 38056.29 32.31 0.050 0.007 0.92-0.84 771 26 26 100.0 29.7 41367.70 40.23 0.062 0.008 0.84-0.78 749 26 26 100.0 28.8 24146.12 25.31 0.065 0.009 0.78-0.73 666 27 27 100.0 24.7 13133.80 19.08 0.079 0.014 0.72-0.69 642 26 26 100.0 24.7 14029.73 17.96 0.078 0.015 0.68-0.66 579 27 27 100.0 21.4 14339.38 19.15 0.080 0.015 0.65-0.63 227 30 30 100.0 7.6 7882.94 6.36 0.083 0.035 -------------------------------------------------------------------------------------------- inf-0.63 6334 240 240 100.0 26.4 40313.27 33.75 0.056 0.009 inf-0.65 6112 211 211 100.0 29.0 41559.19 34.77 0.055 0.008 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066111 0.015108 0.006825 ( 0.000009 0.000009 0.000009 ) -0.016198 0.064804 0.013238 ( 0.000009 0.000009 0.000009 ) -0.003573 -0.014463 0.066530 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004646 0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.004637 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000001 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066111 0.015108 0.006825 ( 0.000009 0.000009 0.000009 ) -0.016198 0.064804 0.013238 ( 0.000009 0.000009 0.000009 ) -0.003573 -0.014463 0.066530 ( 0.000007 0.000007 0.000007 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4064(13) 10.4162(14) 10.4038(10) 89.985(10) 89.988(9) 90.009(11) V = 1127.7(2) unit cell: 10.4088(3) 10.4088(3) 10.4088(3) 90.0 90.0 90.0 V = 1127.72(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.138) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.032) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.032) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.032) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.025) Run 7 Omega scan: (-52.000 - -27.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.032) PROFFIT INFO: signal sum: min=-765.0000 max=7910405.0000 PROFFIT INFO: signal sum lp corr: min=-739.5427 max=1266439.5035 PROFFIT INFO: background sum: min=-86.0000 max=8197.0000 PROFFIT INFO: background sum sig2: min=414.0000 max=5764.0000 PROFFIT INFO: num of signal pixels: min=41 max=506 PROFFIT INFO: Inet: min=-1183.2683 max=2026303.2500 PROFFIT INFO: sig(Inet): min=51.9829 max=30723.3379 PROFFIT INFO: Inet/sig(Inet): min=-2.09 max=276.14 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 1102 4396 6628 7880 8498 9870 10722 11250 12040 12572 12708 Percent 8.7 34.6 52.2 62.0 66.9 77.7 84.4 88.5 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 6354 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 6354 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2026303- 130954 635 412522.92 77.68 100.00 129797- 4045 635 29117.79 19.51 100.00 4043- 2067 635 2873.55 7.05 97.01 2063- 1231 635 1588.05 3.96 52.76 1230- 812 635 1003.76 2.33 16.22 811- 540 635 668.52 1.73 8.35 539- 336 635 433.16 1.21 5.04 336- 155 635 243.08 0.70 0.79 155- 19 635 82.79 0.30 0.00 19- -1183 639 -136.29 -0.27 0.00 ------------------------------------------------------------------------------------ 2026303- -1183 6354 44811.42 11.41 37.99 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 635 112315.56 15.81 68.82 1.64- 1.26 635 85270.76 21.24 59.53 1.26- 1.06 635 62271.72 19.13 68.98 1.06- 0.96 635 52715.28 14.30 32.44 0.96- 0.88 635 19976.75 7.74 44.57 0.88- 0.80 635 48289.93 13.57 35.75 0.80- 0.76 635 18317.31 5.74 19.06 0.76- 0.71 635 21006.07 6.84 16.06 0.71- 0.67 635 24513.89 7.99 28.50 0.67- 0.63 639 3695.93 1.81 6.42 ------------------------------------------------------------------------------------ 6.00- 0.63 6354 44811.42 11.41 37.99 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:52:35 2019 Sorting 6354 observations 43 unique observations with > 7.00 F2/sig(F2) 6354 observations in 7 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 24 639 Total number of frames 639 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 15 frame = 1 scale 6354 observations in 7 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 1 44 Total number of frames 44 1533 observations > 7.00 F2/sig(F2) 1533 observations in 7 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 1 44 Total number of frames 44 Removing 'redundancy=1' reflections Average redundancy: 27.3 (Out of 1533 removed 2 = 1531, unique = 56) 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 1531 observations in 7 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 1 44 Total number of frames 44 56 unique data precomputed (should be 56) 56 unique data with 1531 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 27.3 (Out of 1531 removed 0 = 1531, unique = 56) 56 unique data precomputed (should be 56) 56 unique data with 1531 observations RMS deviation of equivalent data = 0.30908 Rint = 0.25228 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24343, wR= 0.33277 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13257, wR= 0.18631, Acormin=0.473, Acormax=1.420, Acor_av=1.004 F test: Probability=1.000, F= 3.360 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12512, wR= 0.17688, Acormin=0.472, Acormax=1.465, Acor_av=0.979 F test: Probability=0.985, F= 1.120 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12446, wR= 0.17712, Acormin=0.534, Acormax=1.536, Acor_av=1.006 F test: Probability=0.549, F= 1.006 Trying model 4 (ne=4, no=1)... Results: Rint= 0.11445, wR= 0.16488, Acormin=0.465, Acormax=1.568, Acor_av=0.985 F test: Probability=0.999, F= 1.188 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09945, wR= 0.14965, Acormin=0.534, Acormax=1.791, Acor_av=1.030 F test: Probability=1.000, F= 1.318 Final absorption model (ne=4, no=3): Rint= 0.09945, Acormin=0.534, Acormax=1.791, Acor_av=1.030 Combined refinement in use Rint: 0.25411 There are 44 active scales (one needs to be fixed) Refinement control: frame scale #32 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 67 pars with 2278 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30908 Using Levenberg-Marquardt: 0.00010 New wR= 0.13116 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25228 with corrections 0.10430 Rint for all data: 0.25411 with corrections 0.10677 5 observations identified as outliers and rejected Cycle 2 wR= 0.11464 Using Levenberg-Marquardt: 0.00001 New wR= 0.08941 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25226 with corrections 0.06531 Rint for all data: 0.25411 with corrections 0.07320 1 observations identified as outliers and rejected Cycle 3 wR= 0.08710 Using Levenberg-Marquardt: 0.00000 New wR= 0.08434 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25263 with corrections 0.06121 Rint for all data: 0.25411 with corrections 0.06915 0 observations identified as outliers and rejected Cycle 4 wR= 0.08434 Using Levenberg-Marquardt: 0.00000 New wR= 0.08270 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25263 with corrections 0.05924 Rint for all data: 0.25411 with corrections 0.06688 0 observations identified as outliers and rejected Cycle 5 wR= 0.08270 Using Levenberg-Marquardt: 0.00000 New wR= 0.08178 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25263 with corrections 0.05786 Rint for all data: 0.25411 with corrections 0.06522 0 observations identified as outliers and rejected Final wR= 0.08178 Final frame scales: Min= 0.7441 Max= 1.2457 Final absorption correction factors: Amin= 0.3270 Amax= 1.6054 PROFFIT INFO: Inet (after scale3 abspack): min=-1108.7568 max=1271248.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=37.5822 max=26253.2676 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/104 6354 reflections read from tmp file 274 reflections are rejected (274 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 2 2 2 3 4 1 2 146 Initial Chi^2= 0.52817 Cycle 1, Chi^2= 1.00416 Current error model SIG(F2)^2 = 65.61*I_RAW + 10.12*I_BACK+(0.03820*)^2 Cycle 2, Chi^2= 1.01338 Current error model SIG(F2)^2 = 81.38*I_RAW + 6.63*I_BACK+(0.02878*)^2 Cycle 3, Chi^2= 1.00901 Current error model SIG(F2)^2 = 88.82*I_RAW + 5.22*I_BACK+(0.02597*)^2 Cycle 4, Chi^2= 1.00360 Current error model SIG(F2)^2 = 91.68*I_RAW + 4.76*I_BACK+(0.02526*)^2 Cycle 5, Chi^2= 1.00114 Current error model SIG(F2)^2 = 92.61*I_RAW + 4.62*I_BACK+(0.02508*)^2 Cycle 6, Chi^2= 1.00033 Current error model SIG(F2)^2 = 92.88*I_RAW + 4.58*I_BACK+(0.02504*)^2 Cycle 7, Chi^2= 1.00009 Current error model SIG(F2)^2 = 92.96*I_RAW + 4.57*I_BACK+(0.02503*)^2 Final Chi^2= 1.00009 Final error model SIG(F2)^2 = 92.96*I_RAW + 4.57*I_BACK+(0.02503*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1271248- 115499 635 378403.35 31.25 100.00 115393- 3441 635 28918.02 12.75 100.00 3441- 1998 635 2654.10 5.97 99.06 1994- 1146 635 1495.73 3.81 62.52 1145- 765 635 937.73 2.69 23.31 765- 512 635 637.26 2.31 13.23 512- 323 635 411.96 1.94 8.50 322- 150 635 237.16 1.46 2.99 150- 19 635 81.34 0.75 0.47 19- -1109 639 -134.56 -0.56 0.00 ------------------------------------------------------------------------------------ 1271248- -1109 6354 41338.08 6.23 40.98 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 635 105517.53 10.24 71.81 1.64- 1.26 635 78699.92 9.39 61.89 1.26- 1.06 635 58305.36 8.52 72.44 1.06- 0.96 635 47363.76 6.41 33.86 0.96- 0.88 635 18121.76 5.03 50.24 0.88- 0.80 635 44525.80 7.23 40.94 0.80- 0.76 635 16706.17 3.80 21.26 0.76- 0.71 635 18940.20 4.74 18.58 0.71- 0.67 635 22016.85 5.28 31.34 0.67- 0.63 639 3422.33 1.70 7.67 ------------------------------------------------------------------------------------ 6.00- 0.63 6354 41338.08 6.23 40.98 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 635 105517.53 10.24 71.81 6.00- 1.26 1270 92108.73 9.82 66.85 6.00- 1.06 1905 80840.94 9.38 68.71 6.00- 0.96 2540 72471.64 8.64 60.00 6.00- 0.88 3175 61601.67 7.92 58.05 6.00- 0.80 3810 58755.69 7.80 55.20 6.00- 0.76 4445 52748.61 7.23 50.35 6.00- 0.71 5080 48522.56 6.92 46.38 6.00- 0.67 5715 45577.48 6.74 44.71 6.00- 0.63 6354 41338.08 6.23 40.98 ------------------------------------------------------------------------------------ 6.00- 0.63 6354 41338.08 6.23 40.98 Scale applied to data: s=0.786628 (maximum obs:1271248.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.065; Rsigma 0.037: data 6354 -> merged 162 With outlier rejection... Rint 0.056; Rsigma 0.038: data 6337 -> merged 162 Rejected total: 17, method kkm 4, method Blessing 13 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626536, 6.009527 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.41 - 1.76 14 14 41.29 100.00 578 1.73 - 1.27 14 14 45.21 100.00 633 1.26 - 1.06 14 14 51.29 100.00 718 1.05 - 0.97 14 14 44.57 100.00 624 0.95 - 0.88 14 14 46.93 100.00 657 0.87 - 0.81 14 14 41.57 100.00 582 0.80 - 0.76 14 14 43.71 100.00 612 0.76 - 0.72 14 14 36.36 100.00 509 0.72 - 0.69 14 14 40.21 100.00 563 0.69 - 0.65 19 19 33.63 100.00 639 --------------------------------------------------------------- 10.41 - 0.65 145 145 42.17 100.00 6115 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:52:34 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.406228 10.415771 10.403789 89.9813 89.9855 90.0082 6334 Reflections read from file xs2212a.hkl 6297 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.21 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3161 0 4181 4170 6297 N (int>3sigma) = 0 0 0 0 1393 0 1843 1813 2619 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.0 30.3 30.8 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.2 6.2 Lattice type: F chosen Volume: 1127.66 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.357 7.358 7.360 119.98 119.96 90.01 Niggli form: a.a = 54.118 b.b = 54.146 c.c = 54.164 b.c = -27.062 a.c = -27.040 a.b = -0.013 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.086 CUBIC F-lattice R(int) = 0.056 [ 6066] Vol = 1127.7 Cell: 10.416 10.406 10.404 89.99 90.02 89.99 Volume: 1127.66 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.055 TETRAGONAL I-lattice R(int) = 0.055 [ 5680] Vol = 563.8 Cell: 7.361 7.362 10.404 90.00 89.98 89.95 Volume: 563.83 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.036 TETRAGONAL I-lattice R(int) = 0.055 [ 5681] Vol = 563.8 Cell: 7.357 7.358 10.416 89.99 89.98 90.01 Volume: 563.83 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.067 TETRAGONAL I-lattice R(int) = 0.055 [ 5680] Vol = 563.8 Cell: 7.362 7.361 10.404 90.02 90.00 90.05 Volume: 563.83 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.032 ORTHORHOMBIC F-lattice R(int) = 0.054 [ 5627] Vol = 1127.7 Cell: 10.404 10.406 10.416 89.99 90.02 89.99 Volume: 1127.66 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.067 ORTHORHOMBIC I-lattice R(int) = 0.054 [ 5607] Vol = 563.8 Cell: 10.404 7.362 7.361 89.95 89.98 90.00 Volume: 563.83 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.026 ORTHORHOMBIC I-lattice R(int) = 0.053 [ 5607] Vol = 563.8 Cell: 7.357 7.358 10.416 90.01 90.02 90.01 Volume: 563.83 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.037 MONOCLINIC I-lattice R(int) = 0.052 [ 5080] Vol = 563.8 Cell: 7.361 10.404 7.362 90.00 90.05 90.02 Volume: 563.83 Matrix:-0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.032 MONOCLINIC I-lattice R(int) = 0.052 [ 5081] Vol = 563.8 Cell: 7.360 10.406 7.362 90.00 90.07 89.98 Volume: 563.83 Matrix: 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.030 MONOCLINIC I-lattice R(int) = 0.052 [ 5080] Vol = 563.8 Cell: 7.362 10.404 7.361 90.02 90.05 90.00 Volume: 563.83 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.023 MONOCLINIC I-lattice R(int) = 0.052 [ 5059] Vol = 563.8 Cell: 7.358 7.357 10.416 89.98 90.01 89.99 Volume: 563.83 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.017 MONOCLINIC I-lattice R(int) = 0.051 [ 5068] Vol = 563.8 Cell: 7.357 7.358 10.416 89.99 90.02 89.99 Volume: 563.83 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.014 MONOCLINIC I-lattice R(int) = 0.051 [ 5081] Vol = 563.8 Cell: 7.357 10.416 7.358 89.99 90.01 89.98 Volume: 563.83 Matrix: 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.040 MONOCLINIC I-lattice R(int) = 0.051 [ 5081] Vol = 563.8 Cell: 7.357 10.416 7.358 90.01 90.01 90.02 Volume: 563.83 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) = 0.047 [ 4020] Vol = 281.9 Cell: 7.357 7.358 7.360 119.98 119.96 90.01 Volume: 281.91 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -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 3161 0 4188 4189 6297 N (int>3sigma) = 0 0 0 0 1393 0 1855 1847 2619 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 30.4 31.6 30.8 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.3 6.2 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.424 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 45 45 474 1236 N I>3s 2 2 2 662 0.0 0.0 -0.0 1.9 0.8 0.8 0.2 5.0 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 0.055 5620 Fd-3m 1 1 227 C N N N N 37 2284 0.056 5682 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415771 10.406228 10.403789 89.9855 90.0187 89.9918 ZERR 5.00 0.001398 0.001328 0.001033 0.0093 0.0096 0.0106 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1141238- 90944 772 760 27 28.1 325087.60 29.08 0.052 0.069 77419- 1789 1201 1198 27 44.4 5211.43 8.04 0.091 0.101 1643- 758 1289 1287 27 47.7 1105.59 2.89 0.226 0.299 750- 314 1310 1310 27 48.5 480.03 1.96 0.371 0.513 312- 79 831 831 27 30.8 196.11 1.10 0.643 1.194 77- -161 951 951 27 35.2 10.39 0.19 0.963 4.170 ------------------------------------------------------------------------------------------- 1141238- -161 6354 6337 162 39.1 40324.20 6.17 0.056 0.072 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-1.27 1216 1209 27 44.8 92806.40 10.05 0.050 0.064 0.029 1.26-0.97 1347 1342 28 47.9 48375.39 6.98 0.052 0.069 0.034 0.95-0.81 1241 1239 28 44.3 32022.55 6.25 0.065 0.090 0.043 0.80-0.73 1096 1096 27 40.6 17586.71 4.22 0.062 0.079 0.056 0.72-0.67 971 970 27 35.9 17932.69 4.47 0.078 0.105 0.064 0.66-0.63 483 481 25 19.2 4295.35 1.84 0.106 0.086 0.121 ------------------------------------------------------------------------------------------------------ inf-0.63 6354 6337 162 39.1 40324.20 6.17 0.056 0.072 0.038 inf-0.65 6129 6113 144 42.5 41560.60 6.32 0.056 0.072 0.037 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-1.27 1209 27 27 100.0 44.8 92806.40 64.02 0.050 0.006 1.26-0.97 1342 28 28 100.0 47.9 48375.39 45.51 0.052 0.006 0.95-0.81 1239 28 28 100.0 44.3 32022.55 41.77 0.065 0.008 0.80-0.73 1096 27 27 100.0 40.6 17586.71 24.41 0.062 0.010 0.72-0.67 970 27 27 100.0 35.9 17932.69 28.50 0.078 0.011 0.66-0.63 481 25 25 100.0 19.2 4295.35 7.88 0.106 0.030 -------------------------------------------------------------------------------------------- inf-0.63 6337 162 162 100.0 39.1 40324.20 39.20 0.056 0.008 inf-0.65 6113 144 144 100.0 42.5 41560.60 40.40 0.056 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 14:58:33 2019) ID: 3668; threads 40; handles 811; mem 514116.00 (1204692.00)kB; time: 1w 5d 1h 9m 21s MEMORY INFO: Memory PF:223.0, Ph:553.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.1,peak PF: 700.2, WS: 470.4, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:225.0, Ph:555.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:503.9,peak PF: 700.2, WS: 472.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 14:58:33 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000013 0.000014 0.000013 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000012 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000014 ) 10.42433 ( 0.00199 ) 10.43788 ( 0.00189 ) 10.40727 ( 0.00219 ) 89.88512 ( 0.01601 ) 89.79539 ( 0.01628 ) 90.20497 ( 0.01517 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 14:58:33 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000013 0.000014 0.000013 ) -0.015931 0.064696 0.013068 ( 0.000012 0.000012 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000014 ) M - matrix: 0.004646 0.000000 -0.000010 ( 0.000002 0.000001 0.000001 ) 0.000000 0.004643 -0.000002 ( 0.000001 0.000002 0.000001 ) -0.000010 -0.000002 0.004648 ( 0.000001 0.000001 0.000002 ) unit cell: 10.424(2) 10.4379(19) 10.407(2) 89.885(16) 89.795(16) 90.205(15) V = 1132.4(4) unit cell: 10.4066(6) 10.4066(6) 10.4066(6) 90.0 90.0 90.0 V = 1127.00(12) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 212 peaks identified as outliers and rejected 212 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 212 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 212 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.17 | 21 | 0.927 ( 0.078) | 0.993 ( 0.110) | 1.047 ( 0.705) | 1.17- 1.01 | 21 | 0.936 ( 0.095) | 0.959 ( 0.170) | 0.858 ( 0.306) | 1.01- 0.89 | 21 | 0.955 ( 0.073) | 1.002 ( 0.117) | 1.203 ( 0.492) | 0.89- 0.83 | 21 | 0.975 ( 0.074) | 1.041 ( 0.147) | 1.174 ( 0.426) | 0.83- 0.72 | 21 | 0.971 ( 0.040) | 0.955 ( 0.110) | 1.267 ( 0.465) | 0.72- 0.64 | 23 | 0.953 ( 0.043) | 0.916 ( 0.074) | 1.266 ( 0.475) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 212 | 0.932 ( 0.179) | 0.941 ( 0.154) | 1.081 ( 0.703) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 175 obs out of 212 (total:212,skipped:0) (82.55%) UB - matrix: 0.066167 0.011575 0.009058 ( 0.000036 0.000046 0.000035 ) -0.013597 0.064715 0.013261 ( 0.000034 0.000043 0.000033 ) -0.006044 -0.014153 0.065555 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004555 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.510(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 183 1 1 1 OTKP changes: 183 1 1 1 No constraint UB - matrix: 0.066482 0.011708 0.008967 ( 0.000034 0.000044 0.000035 ) -0.013668 0.065082 0.013227 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013970 0.065947 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004644 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004568 0.000045 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000045 0.004604 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066482 0.011708 0.008967 ( 0.000034 0.000044 0.000035 ) -0.013668 0.065082 0.013227 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013970 0.065947 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000001 ) UB fit with 185 obs out of 212 (total:212,skipped:0) (87.26%) unit cell: 10.409(5) 10.495(6) 10.454(6) 90.56(5) 90.18(4) 89.67(5) V = 1142(1) unit cell: 10.4524(16) 10.4524(16) 10.4524(16) 90.0 90.0 90.0 V = 1141.9(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.145) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066482 0.011708 0.008967 ( 0.000034 0.000044 0.000035 ) -0.013668 0.065082 0.013227 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013970 0.065947 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004644 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004568 0.000045 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000045 0.004604 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066482 0.011708 0.008967 ( 0.000034 0.000044 0.000035 ) -0.013668 0.065082 0.013227 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013970 0.065947 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000001 ) UB fit with 185 obs out of 212 (total:212,skipped:0) (87.26%) unit cell: 10.409(5) 10.495(6) 10.454(6) 90.56(5) 90.18(4) 89.67(5) V = 1142(1) unit cell: 10.4524(16) 10.4524(16) 10.4524(16) 90.0 90.0 90.0 V = 1141.9(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 195 obs out of 212 (total:212,skipped:0) (91.98%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 217 peaks identified as outliers and rejected 217 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 217 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 217 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.62 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.605 ( 2.396) | 2.60- 1.76 | 22 | 0.834 ( 0.087) | 0.824 ( 0.144) | 0.810 ( 0.416) | 1.76- 1.57 | 22 | 0.851 ( 0.096) | 0.880 ( 0.155) | 0.728 ( 0.323) | 1.57- 1.35 | 22 | 0.921 ( 0.073) | 0.979 ( 0.140) | 1.048 ( 0.494) | 1.35- 1.16 | 22 | 0.954 ( 0.072) | 1.027 ( 0.125) | 1.037 ( 0.673) | 1.16- 1.01 | 22 | 0.912 ( 0.085) | 0.938 ( 0.170) | 0.926 ( 0.394) | 1.00- 0.88 | 22 | 0.968 ( 0.075) | 1.014 ( 0.129) | 1.210 ( 0.501) | 0.88- 0.79 | 22 | 0.981 ( 0.056) | 1.023 ( 0.138) | 1.203 ( 0.380) | 0.79- 0.69 | 22 | 0.977 ( 0.046) | 0.944 ( 0.102) | 1.276 ( 0.475) | 0.69- 0.63 | 19 | 0.947 ( 0.038) | 0.923 ( 0.086) | 1.314 ( 0.479) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 217 | 0.934 ( 0.194) | 0.943 ( 0.159) | 1.113 ( 0.917) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.942 ( 0.063) | 0.979 ( 0.110) | 0.894 ( 0.374) | 1.09- 0.92 | 25 | 0.955 ( 0.078) | 0.981 ( 0.099) | 1.062 ( 0.467) | 0.92- 0.86 | 25 | 0.944 ( 0.067) | 0.942 ( 0.097) | 1.020 ( 0.391) | 0.82- 0.73 | 25 | 0.957 ( 0.050) | 0.911 ( 0.086) | 1.356 ( 0.420) | 0.73- 0.63 | 28 | 0.929 ( 0.038) | 0.881 ( 0.096) | 1.353 ( 0.467) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 253 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.063 ( 0.485) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.156) HKL list info: 1283 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 192 peaks identified as outliers and rejected 192 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 192 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 192 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.97 | 19 | 0.842 ( 0.116) | 0.844 ( 0.171) | 0.956 ( 0.449) | 2.63- 1.84 | 19 | 0.822 ( 0.111) | 0.843 ( 0.187) | 0.847 ( 0.504) | 1.84- 1.59 | 19 | 0.842 ( 0.108) | 0.837 ( 0.164) | 0.836 ( 0.354) | 1.59- 1.36 | 19 | 0.936 ( 0.096) | 0.973 ( 0.144) | 0.805 ( 0.268) | 1.36- 1.20 | 19 | 0.950 ( 0.102) | 0.972 ( 0.160) | 0.845 ( 0.330) | 1.20- 1.01 | 19 | 0.995 ( 0.078) | 1.010 ( 0.137) | 1.101 ( 0.434) | 1.01- 0.88 | 19 | 0.998 ( 0.085) | 1.016 ( 0.121) | 1.030 ( 0.364) | 0.88- 0.79 | 19 | 1.037 ( 0.059) | 1.056 ( 0.123) | 0.938 ( 0.316) | 0.79- 0.72 | 19 | 1.031 ( 0.054) | 0.994 ( 0.144) | 1.279 ( 0.526) | 0.70- 0.63 | 21 | 0.975 ( 0.052) | 0.883 ( 0.059) | 1.164 ( 0.415) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 192 | 0.943 ( 0.117) | 0.942 ( 0.164) | 0.982 ( 0.432) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) UB - matrix: 0.065810 0.015591 0.006262 ( 0.000023 0.000019 0.000022 ) -0.016403 0.064531 0.013131 ( 0.000023 0.000020 0.000022 ) -0.002751 -0.014148 0.066421 ( 0.000026 0.000022 0.000025 ) M - matrix: 0.004608 0.000006 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004607 0.000005 ( 0.000002 0.000003 0.000002 ) 0.000014 0.000005 0.004623 ( 0.000002 0.000002 0.000003 ) unit cell: 10.450(3) 10.450(3) 10.432(4) 90.07(3) 90.17(3) 90.08(3) V = 1139.1(6) OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 1279 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 190 peaks identified as outliers and rejected 190 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 190 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 190 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 3.00 | 19 | 0.846 ( 0.114) | 0.847 ( 0.168) | 0.873 ( 0.501) | 2.99- 2.00 | 19 | 0.802 ( 0.108) | 0.800 ( 0.186) | 0.843 ( 0.452) | 1.84- 1.59 | 19 | 0.842 ( 0.097) | 0.828 ( 0.155) | 0.880 ( 0.351) | 1.59- 1.36 | 19 | 0.948 ( 0.083) | 0.983 ( 0.140) | 0.851 ( 0.258) | 1.36- 1.19 | 19 | 0.950 ( 0.094) | 0.960 ( 0.152) | 0.768 ( 0.211) | 1.19- 1.00 | 19 | 1.018 ( 0.060) | 1.041 ( 0.127) | 1.085 ( 0.364) | 1.00- 0.88 | 19 | 1.010 ( 0.085) | 1.031 ( 0.121) | 1.045 ( 0.373) | 0.88- 0.78 | 19 | 1.033 ( 0.056) | 1.044 ( 0.117) | 0.953 ( 0.322) | 0.78- 0.69 | 19 | 1.031 ( 0.055) | 1.004 ( 0.165) | 1.278 ( 0.531) | 0.69- 0.63 | 19 | 0.970 ( 0.050) | 0.876 ( 0.055) | 1.127 ( 0.364) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 190 | 0.945 ( 0.116) | 0.942 ( 0.169) | 0.970 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Creating background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb PROFFITPEAK info: 168 peaks in the peak location table UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 No constraint UB - matrix: 0.066110 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) Constraint UB - matrix: 0.066110 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004619 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004619 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004619 ( 0.000000 0.000000 0.000002 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) unit cell: 10.426(2) 10.426(2) 10.426(2) 90.0 90.0 90.0 V = 1133.2(4) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) UB - matrix: 0.066109 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 No constraint UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) Constraint UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004617 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004617 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004617 ( 0.000000 0.000000 0.000002 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) unit cell: 10.427(2) 10.427(2) 10.427(2) 90.0 90.0 90.0 V = 1133.7(4) 106 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) Constraint UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004617 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004617 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004617 ( 0.000000 0.000000 0.000002 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) unit cell: 10.427(2) 10.427(2) 10.427(2) 90.0 90.0 90.0 V = 1133.7(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) 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= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 100 peaks identified as outliers and rejected 100 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 100 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 100 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 2.37 | 10 | 0.824 ( 0.107) | 0.789 ( 0.168) | 0.948 ( 0.526) | 2.13- 1.65 | 10 | 0.887 ( 0.099) | 0.902 ( 0.146) | 0.800 ( 0.370) | 1.64- 1.46 | 10 | 0.917 ( 0.142) | 0.896 ( 0.234) | 0.948 ( 0.416) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.161) | 1.038 ( 0.459) | 1.23- 1.11 | 10 | 1.014 ( 0.089) | 1.022 ( 0.172) | 1.004 ( 0.500) | 1.11- 1.00 | 10 | 0.988 ( 0.107) | 1.011 ( 0.206) | 0.971 ( 0.392) | 1.00- 0.89 | 10 | 1.016 ( 0.106) | 1.093 ( 0.173) | 0.829 ( 0.141) | 0.89- 0.86 | 10 | 0.995 ( 0.094) | 1.038 ( 0.093) | 1.245 ( 0.487) | 0.82- 0.73 | 10 | 1.072 ( 0.046) | 1.130 ( 0.142) | 0.868 ( 0.108) | 0.72- 0.64 | 10 | 1.031 ( 0.064) | 1.069 ( 0.171) | 1.233 ( 0.765) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 0.64 | 100 | 0.972 ( 0.121) | 0.995 ( 0.197) | 0.988 ( 0.476) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) UB - matrix: 0.065966 0.015448 0.005965 ( 0.000053 0.000028 0.000028 ) -0.016426 0.064502 0.013369 ( 0.000054 0.000029 0.000028 ) -0.002418 -0.014553 0.066425 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004627 -0.000005 0.000013 ( 0.000007 0.000004 0.000003 ) -0.000005 0.004611 -0.000012 ( 0.000004 0.000004 0.000002 ) 0.000013 -0.000012 0.004627 ( 0.000003 0.000002 0.000002 ) unit cell: 10.427(8) 10.446(5) 10.428(3) 89.85(3) 90.16(4) 89.93(5) V = 1136(1) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) 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! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 101 peaks identified as outliers and rejected 101 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 101 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 101 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.38 | 10 | 0.825 ( 0.107) | 0.790 ( 0.169) | 1.019 ( 0.527) | 2.13- 1.64 | 10 | 0.860 ( 0.122) | 0.859 ( 0.190) | 0.860 ( 0.389) | 1.64- 1.46 | 10 | 0.944 ( 0.113) | 0.943 ( 0.190) | 0.940 ( 0.402) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.160) | 1.023 ( 0.449) | 1.23- 1.11 | 10 | 1.002 ( 0.107) | 0.995 ( 0.210) | 0.997 ( 0.506) | 1.09- 1.00 | 10 | 1.034 ( 0.082) | 1.115 ( 0.140) | 0.886 ( 0.284) | 0.97- 0.88 | 10 | 0.989 ( 0.091) | 1.159 ( 0.229) | 0.740 ( 0.286) | 0.88- 0.86 | 10 | 1.009 ( 0.084) | 1.059 ( 0.096) | 1.119 ( 0.453) | 0.82- 0.73 | 10 | 1.071 ( 0.046) | 1.128 ( 0.142) | 0.868 ( 0.110) | 0.72- 0.63 | 11 | 1.023 ( 0.066) | 1.042 ( 0.168) | 1.108 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.63 | 101 | 0.974 ( 0.119) | 1.009 ( 0.206) | 0.958 ( 0.416) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.2 | 149 | 0.993 ( 0.042) | 1.040 ( 0.070) | 1.117 ( 0.495) | 10.3-15.0 | 149 | 0.997 ( 0.049) | 1.053 ( 0.072) | 1.103 ( 0.507) | 15.0-19.3 | 149 | 0.997 ( 0.176) | 1.039 ( 0.102) | 1.124 ( 0.927) | 19.3-23.6 | 149 | 0.973 ( 0.066) | 1.013 ( 0.087) | 0.944 ( 0.405) | 23.6-27.5 | 149 | 0.975 ( 0.070) | 1.016 ( 0.117) | 0.963 ( 0.459) | 27.5-32.5 | 149 | 0.948 ( 0.085) | 0.969 ( 0.119) | 0.920 ( 0.430) | 32.5-36.3 | 149 | 0.923 ( 0.154) | 0.912 ( 0.149) | 1.065 ( 0.645) | 36.3-38.9 | 149 | 0.892 ( 0.110) | 0.880 ( 0.242) | 0.986 ( 0.449) | 38.9-41.9 | 149 | 0.899 ( 0.104) | 0.855 ( 0.155) | 0.999 ( 0.452) | 41.9-50.2 | 152 | 0.867 ( 0.127) | 0.792 ( 0.149) | 0.944 ( 0.438) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.2 | 1493 | 0.946 ( 0.116) | 0.957 ( 0.161) | 1.016 ( 0.547) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.14 e2 dimension: a=-0.0068 b=1.24 e3 dimension: a=-0.0004 b=1.12 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 5011 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 14:58:54 2019 PROFFITMAIN - Started at Wed Aug 21 14:58:54 2019 OTKP changes: 1165 2 6 7 OTKP changes: 1165 2 6 7 OTKP changes: 1165 2 6 7 No constraint UB - matrix: 0.066134 0.015130 0.006691 ( 0.000012 0.000013 0.000013 ) -0.016239 0.064851 0.013218 ( 0.000012 0.000012 0.000012 ) -0.003577 -0.014472 0.066513 ( 0.000014 0.000015 0.000014 ) M - matrix: 0.004650 -0.000001 -0.000010 ( 0.000002 0.000001 0.000001 ) -0.000001 0.004644 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000010 -0.000004 0.004643 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066134 0.015130 0.006691 ( 0.000012 0.000013 0.000013 ) -0.016239 0.064851 0.013218 ( 0.000012 0.000012 0.000012 ) -0.003577 -0.014472 0.066513 ( 0.000014 0.000015 0.000014 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 1194 obs out of 1493 (total:1493,skipped:0) (79.97%) unit cell: 10.4015(19) 10.4084(19) 10.409(2) 89.949(16) 89.876(16) 89.991(15) V = 1126.9(4) unit cell: 10.4063(6) 10.4063(6) 10.4063(6) 90.0 90.0 90.0 V = 1126.90(12) *** 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 184 obs out of 217 (total:217,skipped:0) (84.79%) UB - matrix: 0.066495 0.011705 0.008959 ( 0.000033 0.000043 0.000036 ) -0.013692 0.065050 0.013254 ( 0.000031 0.000040 0.000034 ) -0.006040 -0.013933 0.065919 ( 0.000035 0.000045 0.000038 ) M - matrix: 0.004645 -0.000028 0.000016 ( 0.000005 0.000004 0.000003 ) -0.000028 0.004563 0.000049 ( 0.000004 0.000005 0.000004 ) 0.000016 0.000049 0.004601 ( 0.000003 0.000004 0.000005 ) unit cell: 10.407(5) 10.502(6) 10.457(6) 90.61(5) 90.20(4) 89.65(4) V = 1143(1) OTKP changes: 186 1 1 1 OTKP changes: 186 1 1 1 No constraint UB - matrix: 0.066507 0.011709 0.008953 ( 0.000033 0.000043 0.000036 ) -0.013715 0.065060 0.013257 ( 0.000032 0.000041 0.000034 ) -0.006045 -0.013929 0.065951 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004648 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004564 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004605 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066507 0.011709 0.008953 ( 0.000033 0.000043 0.000036 ) -0.013715 0.065060 0.013257 ( 0.000032 0.000041 0.000034 ) -0.006045 -0.013929 0.065951 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000002 ) UB fit with 187 obs out of 217 (total:217,skipped:0) (86.18%) unit cell: 10.404(5) 10.500(6) 10.452(6) 90.61(5) 90.19(4) 89.63(4) V = 1142(1) unit cell: 10.4520(19) 10.4520(19) 10.4520(19) 90.0 90.0 90.0 V = 1141.8(3) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.131) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066507 0.011709 0.008953 ( 0.000033 0.000043 0.000036 ) -0.013715 0.065060 0.013257 ( 0.000032 0.000041 0.000034 ) -0.006045 -0.013929 0.065951 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004648 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004564 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004605 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066507 0.011709 0.008953 ( 0.000033 0.000043 0.000036 ) -0.013715 0.065060 0.013257 ( 0.000032 0.000041 0.000034 ) -0.006045 -0.013929 0.065951 ( 0.000035 0.000046 0.000038 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000002 ) UB fit with 187 obs out of 217 (total:217,skipped:0) (86.18%) unit cell: 10.404(5) 10.500(6) 10.452(6) 90.61(5) 90.19(4) 89.63(4) V = 1142(1) unit cell: 10.4520(19) 10.4520(19) 10.4520(19) 90.0 90.0 90.0 V = 1141.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 201 obs out of 217 (total:217,skipped:0) (92.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068153 -0.000275 0.000134 ( 0.000029 0.000037 0.000030 ) -0.000070 0.067615 0.000622 ( 0.000032 0.000040 0.000032 ) -0.000037 -0.000064 0.067961 ( 0.000023 0.000030 0.000024 ) M - matrix: 0.004645 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004572 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004619 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068153 -0.000275 0.000134 ( 0.000029 0.000037 0.000030 ) -0.000070 0.067615 0.000622 ( 0.000032 0.000040 0.000032 ) -0.000037 -0.000064 0.067961 ( 0.000023 0.000030 0.000024 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 202 obs out of 217 (total:217,skipped:0) (93.09%) unit cell: 10.408(4) 10.491(6) 10.437(4) 90.47(4) 90.08(3) 89.71(4) V = 1139.5(9) unit cell: 10.4448(13) 10.4448(13) 10.4448(13) 90.0 90.0 90.0 V = 1139.5(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.066335 0.014184 0.006779 ( 0.000027 0.000035 0.000035 ) -0.015583 0.064701 0.012861 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014192 0.066901 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000010 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000010 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 No constraint UB - matrix: 0.066339 0.014183 0.006781 ( 0.000027 0.000035 0.000035 ) -0.015580 0.064696 0.012864 ( 0.000017 0.000023 0.000023 ) -0.004082 -0.014194 0.066898 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066339 0.014183 0.006781 ( 0.000027 0.000035 0.000035 ) -0.015580 0.064696 0.012864 ( 0.000017 0.000023 0.000023 ) -0.004082 -0.014194 0.066898 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.390(4) 10.472(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.3(7) unit cell: 10.4075(5) 10.4075(5) 10.4075(5) 90.0 90.0 90.0 V = 1127.29(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.005) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066339 0.014183 0.006781 ( 0.000027 0.000035 0.000035 ) -0.015580 0.064696 0.012864 ( 0.000017 0.000023 0.000023 ) -0.004082 -0.014194 0.066898 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066339 0.014183 0.006781 ( 0.000027 0.000035 0.000035 ) -0.015580 0.064696 0.012864 ( 0.000017 0.000023 0.000023 ) -0.004082 -0.014194 0.066898 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.390(4) 10.472(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.3(7) unit cell: 10.4075(5) 10.4075(5) 10.4075(5) 90.0 90.0 90.0 V = 1127.29(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068241 -0.000106 -0.000274 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067886 -0.000162 ( 0.000017 0.000022 0.000022 ) -0.000012 0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000006 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000006 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068241 -0.000106 -0.000274 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067886 -0.000162 ( 0.000017 0.000022 0.000022 ) -0.000012 0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.394(3) 10.448(3) 10.373(3) 89.87(2) 89.76(3) 89.93(3) V = 1126.6(6) unit cell: 10.4052(5) 10.4052(5) 10.4052(5) 90.0 90.0 90.0 V = 1126.56(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065885 0.015205 0.006803 ( 0.000019 0.000013 0.000019 ) -0.016070 0.064777 0.013235 ( 0.000017 0.000012 0.000016 ) -0.003638 -0.014512 0.066498 ( 0.000021 0.000015 0.000021 ) M - matrix: 0.004612 0.000014 -0.000006 ( 0.000003 0.000001 0.000002 ) 0.000014 0.004638 -0.000004 ( 0.000001 0.000002 0.000002 ) -0.000006 -0.000004 0.004643 ( 0.000002 0.000002 0.000003 ) unit cell: 10.444(3) 10.415(2) 10.409(3) 89.948(19) 89.92(2) 90.169(18) V = 1132.3(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065926 0.015220 0.006786 ( 0.000019 0.000013 0.000019 ) -0.016117 0.064837 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003641 -0.014463 0.066564 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004619 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004645 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004652 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065926 0.015220 0.006786 ( 0.000019 0.000013 0.000019 ) -0.016117 0.064837 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003641 -0.014463 0.066564 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.436(3) 10.4077(19) 10.399(3) 89.997(18) 89.89(2) 90.137(18) V = 1129.5(5) unit cell: 10.4143(5) 10.4143(5) 10.4143(5) 90.0 90.0 90.0 V = 1129.51(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.045) HKL list info: 1275 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065926 0.015220 0.006786 ( 0.000019 0.000013 0.000019 ) -0.016117 0.064837 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003641 -0.014463 0.066564 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004619 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004645 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004652 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065926 0.015220 0.006786 ( 0.000019 0.000013 0.000019 ) -0.016117 0.064837 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003641 -0.014463 0.066564 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.436(3) 10.4077(19) 10.399(3) 89.997(18) 89.89(2) 90.137(18) V = 1129.5(5) unit cell: 10.4143(5) 10.4143(5) 10.4143(5) 90.0 90.0 90.0 V = 1129.51(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065926 0.015220 0.006786 ( 0.000019 0.000013 0.000019 ) -0.016117 0.064837 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003641 -0.014463 0.066564 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004619 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004645 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004652 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065926 0.015220 0.006786 ( 0.000019 0.000013 0.000019 ) -0.016117 0.064837 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003641 -0.014463 0.066564 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.436(3) 10.4077(19) 10.399(3) 89.997(18) 89.89(2) 90.137(18) V = 1129.5(5) unit cell: 10.4143(5) 10.4143(5) 10.4143(5) 90.0 90.0 90.0 V = 1129.51(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066117 0.015252 0.006585 ( 0.000015 0.000020 0.000017 ) -0.016348 0.064736 0.012924 ( 0.000012 0.000016 0.000013 ) -0.003357 -0.014202 0.066510 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004650 -0.000002 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000002 0.004625 -0.000007 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000007 0.004634 ( 0.000001 0.000001 0.000002 ) unit cell: 10.402(2) 10.430(2) 10.4196(19) 89.908(16) 90.010(17) 89.972(19) V = 1130.4(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066144 0.015264 0.006528 ( 0.000013 0.000018 0.000015 ) -0.016362 0.064780 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003346 -0.014170 0.066601 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004654 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004630 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004646 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066144 0.015264 0.006528 ( 0.000013 0.000018 0.000015 ) -0.016362 0.064780 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003346 -0.014170 0.066601 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.397(2) 10.424(2) 10.4059(18) 89.945(16) 89.961(15) 89.964(18) V = 1127.8(4) unit cell: 10.4090(5) 10.4090(5) 10.4090(5) 90.0 90.0 90.0 V = 1127.79(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.045) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066144 0.015264 0.006528 ( 0.000013 0.000018 0.000015 ) -0.016362 0.064780 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003346 -0.014170 0.066601 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004654 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004630 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004646 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066144 0.015264 0.006528 ( 0.000013 0.000018 0.000015 ) -0.016362 0.064780 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003346 -0.014170 0.066601 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.397(2) 10.424(2) 10.4059(18) 89.945(16) 89.961(15) 89.964(18) V = 1127.8(4) unit cell: 10.4090(5) 10.4090(5) 10.4090(5) 90.0 90.0 90.0 V = 1127.79(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068205 -0.000039 -0.000036 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068061 -0.000053 ( 0.000013 0.000018 0.000015 ) 0.000008 0.000010 0.068165 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004652 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004632 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004646 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068205 -0.000039 -0.000036 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068061 -0.000053 ( 0.000013 0.000018 0.000015 ) 0.000008 0.000010 0.068165 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.3996(16) 10.422(3) 10.4056(15) 89.964(16) 89.976(13) 89.968(17) V = 1127.8(4) unit cell: 10.4089(5) 10.4089(5) 10.4089(5) 90.0 90.0 90.0 V = 1127.76(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 263 obs out of 271 (total:271,skipped:0) (97.05%) UB - matrix: 0.065972 0.015338 0.006327 ( 0.000016 0.000012 0.000013 ) -0.016382 0.064793 0.013411 ( 0.000020 0.000015 0.000015 ) -0.002944 -0.014576 0.066480 ( 0.000021 0.000016 0.000016 ) M - matrix: 0.004629 -0.000007 0.000002 ( 0.000002 0.000002 0.000002 ) -0.000007 0.004646 -0.000003 ( 0.000002 0.000002 0.000001 ) 0.000002 -0.000003 0.004640 ( 0.000002 0.000001 0.000002 ) unit cell: 10.425(2) 10.406(2) 10.413(2) 89.963(19) 90.02(2) 89.917(19) V = 1129.7(5) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.066040 0.015383 0.006330 ( 0.000016 0.000012 0.000013 ) -0.016390 0.064837 0.013379 ( 0.000018 0.000013 0.000014 ) -0.002874 -0.014635 0.066553 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004638 -0.000005 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004655 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066040 0.015383 0.006330 ( 0.000016 0.000012 0.000013 ) -0.016390 0.064837 0.013379 ( 0.000018 0.000013 0.000014 ) -0.002874 -0.014635 0.066553 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.415(2) 10.396(2) 10.4035(18) 89.887(15) 90.092(17) 89.941(18) V = 1126.5(4) unit cell: 10.4050(5) 10.4050(5) 10.4050(5) 90.0 90.0 90.0 V = 1126.47(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.045) HKL list info: 1297 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066040 0.015383 0.006330 ( 0.000016 0.000012 0.000013 ) -0.016390 0.064837 0.013379 ( 0.000018 0.000013 0.000014 ) -0.002874 -0.014635 0.066553 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004638 -0.000005 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004655 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066040 0.015383 0.006330 ( 0.000016 0.000012 0.000013 ) -0.016390 0.064837 0.013379 ( 0.000018 0.000013 0.000014 ) -0.002874 -0.014635 0.066553 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.415(2) 10.396(2) 10.4035(18) 89.887(15) 90.092(17) 89.941(18) V = 1126.5(4) unit cell: 10.4050(5) 10.4050(5) 10.4050(5) 90.0 90.0 90.0 V = 1126.47(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068110 -0.000094 0.000071 ( 0.000017 0.000013 0.000014 ) 0.000059 0.068195 -0.000091 ( 0.000014 0.000010 0.000011 ) -0.000018 0.000009 0.068171 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004639 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004651 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004647 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068110 -0.000094 0.000071 ( 0.000017 0.000013 0.000014 ) 0.000059 0.068195 -0.000091 ( 0.000014 0.000010 0.000011 ) -0.000018 0.000009 0.068171 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.414(3) 10.4011(16) 10.4046(18) 89.931(13) 90.044(17) 89.971(16) V = 1127.0(4) unit cell: 10.4066(5) 10.4066(5) 10.4066(5) 90.0 90.0 90.0 V = 1127.01(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 158 obs out of 190 (total:190,skipped:0) (83.16%) UB - matrix: 0.066084 0.015492 0.006322 ( 0.000029 0.000027 0.000028 ) -0.016500 0.064860 0.013030 ( 0.000030 0.000027 0.000029 ) -0.003362 -0.014171 0.066476 ( 0.000054 0.000050 0.000052 ) M - matrix: 0.004651 0.000001 -0.000021 ( 0.000004 0.000003 0.000004 ) 0.000001 0.004648 0.000001 ( 0.000003 0.000004 0.000004 ) -0.000021 0.000001 0.004629 ( 0.000004 0.000004 0.000007 ) unit cell: 10.401(4) 10.404(4) 10.426(8) 90.01(5) 89.74(5) 90.02(3) V = 1128(1) OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 No constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004638 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.415(3) 10.421(3) 10.405(2) 89.85(2) 90.17(2) 90.10(2) V = 1129.2(5) unit cell: 10.4134(7) 10.4134(7) 10.4134(7) 90.0 90.0 90.0 V = 1129.23(13) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) HKL list info: 1266 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004638 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.415(3) 10.421(3) 10.405(2) 89.85(2) 90.17(2) 90.10(2) V = 1129.2(5) unit cell: 10.4134(7) 10.4134(7) 10.4134(7) 90.0 90.0 90.0 V = 1129.23(13) 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! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: 0.068131 0.000083 0.000194 ( 0.000020 0.000016 0.000019 ) -0.000013 0.068074 -0.000160 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068166 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000005 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000005 0.004634 -0.000011 ( 0.000002 0.000002 0.000002 ) 0.000013 -0.000011 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.068131 0.000083 0.000194 ( 0.000020 0.000016 0.000019 ) -0.000013 0.068074 -0.000160 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068166 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.411(3) 10.420(3) 10.4055(18) 89.867(19) 90.161(19) 90.06(2) V = 1128.7(5) unit cell: 10.4120(7) 10.4120(7) 10.4120(7) 90.0 90.0 90.0 V = 1128.75(12) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.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= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) UB - matrix: 0.066050 0.015406 0.005978 ( 0.000054 0.000029 0.000029 ) -0.016526 0.064607 0.013496 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014551 0.066437 ( 0.000034 0.000018 0.000018 ) M - matrix: 0.004641 -0.000015 0.000013 ( 0.000007 0.000003 0.000003 ) -0.000015 0.004623 -0.000003 ( 0.000003 0.000002 0.000002 ) 0.000013 -0.000003 0.004632 ( 0.000003 0.000002 0.000002 ) unit cell: 10.411(8) 10.432(3) 10.422(3) 89.97(2) 90.15(4) 89.81(4) V = 1132.0(10) OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 No constraint UB - matrix: 0.066056 0.015404 0.005976 ( 0.000054 0.000029 0.000029 ) -0.016530 0.064613 0.013504 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014547 0.066441 ( 0.000035 0.000019 0.000018 ) M - matrix: 0.004642 -0.000016 0.000012 ( 0.000007 0.000003 0.000003 ) -0.000016 0.004624 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000012 -0.000002 0.004632 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066056 0.015404 0.005976 ( 0.000054 0.000029 0.000029 ) -0.016530 0.064613 0.013504 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014547 0.066441 ( 0.000035 0.000019 0.000018 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.410(8) 10.431(3) 10.421(3) 89.98(2) 90.15(4) 89.81(4) V = 1131.7(10) unit cell: 10.4209(11) 10.4209(11) 10.4209(11) 90.0 90.0 90.0 V = 1131.7(2) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 674 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066056 0.015404 0.005976 ( 0.000054 0.000029 0.000029 ) -0.016530 0.064613 0.013504 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014547 0.066441 ( 0.000035 0.000019 0.000018 ) M - matrix: 0.004642 -0.000016 0.000012 ( 0.000007 0.000003 0.000003 ) -0.000016 0.004624 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000012 -0.000002 0.004632 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066056 0.015404 0.005976 ( 0.000054 0.000029 0.000029 ) -0.016530 0.064613 0.013504 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014547 0.066441 ( 0.000035 0.000019 0.000018 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.410(8) 10.431(3) 10.421(3) 89.98(2) 90.15(4) 89.81(4) V = 1131.7(10) unit cell: 10.4209(11) 10.4209(11) 10.4209(11) 90.0 90.0 90.0 V = 1131.7(2) 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 7) ******* No constraint UB - matrix: 0.068141 -0.000220 0.000186 ( 0.000054 0.000029 0.000028 ) -0.000007 0.067997 -0.000026 ( 0.000030 0.000016 0.000016 ) 0.000000 -0.000002 0.068061 ( 0.000035 0.000019 0.000019 ) M - matrix: 0.004643 -0.000015 0.000013 ( 0.000007 0.000003 0.000003 ) -0.000015 0.004624 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000013 -0.000002 0.004632 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.068141 -0.000220 0.000186 ( 0.000054 0.000029 0.000028 ) -0.000007 0.067997 -0.000026 ( 0.000030 0.000016 0.000016 ) 0.000000 -0.000002 0.068061 ( 0.000035 0.000019 0.000019 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.409(8) 10.431(2) 10.422(3) 89.98(2) 90.16(4) 89.81(3) V = 1131.6(10) unit cell: 10.4207(11) 10.4207(11) 10.4207(11) 90.0 90.0 90.0 V = 1131.6(2) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 56.89 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068152 0.000008 -0.000030 ( 0.000009 0.000009 0.000009 ) -0.000002 0.068085 -0.000009 ( 0.000009 0.000009 0.000009 ) 0.000028 -0.000019 0.068164 ( 0.000007 0.000006 0.000007 ) M - matrix: 0.004645 0.000000 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000000 0.004636 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000000 -0.000002 0.004646 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068152 0.000008 -0.000030 ( 0.000009 0.000009 0.000009 ) -0.000002 0.068085 -0.000009 ( 0.000009 0.000009 0.000009 ) 0.000028 -0.000019 0.068164 ( 0.000007 0.000006 0.000007 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) UB fit with 1470 obs out of 1493 (total:1493,skipped:0) (98.46%) unit cell: 10.4076(13) 10.4179(13) 10.4058(10) 89.977(9) 89.998(9) 90.006(10) V = 1128.2(2) unit cell: 10.4104(3) 10.4104(3) 10.4104(3) 90.0 90.0 90.0 V = 1128.25(6) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 179 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_7.rrpprof 6582 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 14:59:04 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.131) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.005) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.045) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.045) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.045) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) PROFFIT INFO: signal sum: min=-743.0000 max=7943242.0000 PROFFIT INFO: signal sum lp corr: min=-736.9381 max=1263717.5630 PROFFIT INFO: background sum: min=-80.0000 max=8164.0000 PROFFIT INFO: background sum sig2: min=440.0000 max=5768.0000 PROFFIT INFO: num of signal pixels: min=41 max=513 PROFFIT INFO: Inet: min=-1179.1011 max=2021948.2500 PROFFIT INFO: sig(Inet): min=52.2344 max=30724.9844 PROFFIT INFO: Inet/sig(Inet): min=-1.97 max=276.25 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 577 2261 3419 4080 4403 5114 5555 5828 6234 6511 6582 Percent 8.8 34.4 51.9 62.0 66.9 77.7 84.4 88.5 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 6582 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 6582 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2021948- 131112 658 417401.24 77.99 100.00 130948- 4053 658 28870.91 19.38 100.00 4051- 2109 658 2900.51 7.06 97.11 2109- 1246 658 1606.68 3.95 52.74 1246- 820 658 1013.72 2.35 16.26 819- 547 658 675.77 1.73 8.36 547- 342 658 440.60 1.23 5.17 341- 157 658 247.50 0.72 0.61 157- 19 658 82.61 0.30 0.00 19- -1179 660 -138.10 -0.27 0.00 ------------------------------------------------------------------------------------ 2021948- -1179 6582 45296.33 11.44 38.01 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 658 111403.63 15.65 68.09 1.64- 1.26 658 88560.72 21.42 58.97 1.26- 1.06 658 68565.32 20.20 69.15 1.06- 0.96 658 47981.41 13.34 31.61 0.96- 0.88 658 23190.64 8.58 46.05 0.88- 0.80 658 45096.22 12.73 34.80 0.80- 0.75 658 18975.10 5.88 19.76 0.75- 0.71 658 20981.93 6.82 16.41 0.71- 0.67 658 24745.92 8.03 29.03 0.67- 0.63 660 3589.21 1.78 6.36 ------------------------------------------------------------------------------------ 6.00- 0.63 6582 45296.33 11.44 38.01 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:59:04 2019 Sorting 6582 observations 53 unique observations with > 7.00 F2/sig(F2) 6582 observations in 7 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 Total number of frames 661 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 13 frame = 1 scale 6582 observations in 7 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 3 52 Total number of frames 52 1591 observations > 7.00 F2/sig(F2) 1591 observations in 7 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 3 52 Total number of frames 52 Removing 'redundancy=1' reflections Average redundancy: 23.0 (Out of 1591 removed 7 = 1584, unique = 69) 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 1584 observations in 7 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 3 52 Total number of frames 52 69 unique data precomputed (should be 69) 69 unique data with 1584 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.0 (Out of 1584 removed 0 = 1584, unique = 69) 69 unique data precomputed (should be 69) 69 unique data with 1584 observations RMS deviation of equivalent data = 0.31402 Rint = 0.25541 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24657, wR= 0.33980 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13716, wR= 0.18918, Acormin=0.470, Acormax=1.435, Acor_av=0.996 F test: Probability=1.000, F= 3.221 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13420, wR= 0.18278, Acormin=0.477, Acormax=1.483, Acor_av=0.980 F test: Probability=0.790, F= 1.042 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13048, wR= 0.18060, Acormin=0.549, Acormax=1.546, Acor_av=1.002 F test: Probability=0.965, F= 1.098 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12468, wR= 0.17183, Acormin=0.491, Acormax=1.572, Acor_av=0.988 F test: Probability=0.957, F= 1.093 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10562, wR= 0.15288, Acormin=0.561, Acormax=1.829, Acor_av=1.036 F test: Probability=1.000, F= 1.387 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12344, wR= 0.17347, Acormin=0.425, Acormax=1.635, Acor_av=0.984 F test: Probability=0.000, F= 0.731 Trying model 7 (ne=6, no=1)... Results: Rint= 0.11967, wR= 0.16645, Acormin=0.450, Acormax=1.620, Acor_av=0.978 F test: Probability=0.000, F= 0.776 Trying model 8 (ne=6, no=3)... Results: Rint= 0.10109, wR= 0.14935, Acormin=0.533, Acormax=1.838, Acor_av=1.025 F test: Probability=0.935, F= 1.082 Trying model 9 (ne=6, no=5)... Results: Rint= 0.15066, wR= 0.19589, Acormin=0.115, Acormax=1.112, Acor_av=0.532 F test: Probability=0.000, F= 0.484 Final absorption model (ne=4, no=3): Rint= 0.10562, Acormin=0.561, Acormax=1.829, Acor_av=1.036 Combined refinement in use Rint: 0.25726 There are 52 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 75 pars with 2850 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31402 Using Levenberg-Marquardt: 0.00010 New wR= 0.11996 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25541 with corrections 0.09656 Rint for all data: 0.25726 with corrections 0.09913 5 observations identified as outliers and rejected Cycle 2 wR= 0.10337 Using Levenberg-Marquardt: 0.00001 New wR= 0.08628 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25546 with corrections 0.05921 Rint for all data: 0.25726 with corrections 0.06571 1 observations identified as outliers and rejected Cycle 3 wR= 0.08459 Using Levenberg-Marquardt: 0.00000 New wR= 0.08246 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25526 with corrections 0.05787 Rint for all data: 0.25726 with corrections 0.06497 0 observations identified as outliers and rejected Cycle 4 wR= 0.08246 Using Levenberg-Marquardt: 0.00000 New wR= 0.08199 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25526 with corrections 0.05684 Rint for all data: 0.25726 with corrections 0.06371 2 observations identified as outliers and rejected Cycle 5 wR= 0.07669 Using Levenberg-Marquardt: 0.00000 New wR= 0.07760 Using Levenberg-Marquardt: 0.00000 New wR= 0.07760 Using Levenberg-Marquardt: 0.00000 New wR= 0.07760 Using Levenberg-Marquardt: 0.00001 New wR= 0.07760 Using Levenberg-Marquardt: 0.00010 New wR= 0.07759 Using Levenberg-Marquardt: 0.00100 New wR= 0.07758 Using Levenberg-Marquardt: 0.01000 New wR= 0.07749 Using Levenberg-Marquardt: 0.10000 New wR= 0.07696 Using Levenberg-Marquardt: 1.00000 New wR= 0.07636 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25328 with corrections 0.05345 Rint for all data: 0.25726 with corrections 0.06149 2 observations identified as outliers and rejected Final wR= 0.07636 Final frame scales: Min= 0.7452 Max= 1.3642 Final absorption correction factors: Amin= 0.3050 Amax= 1.6379 PROFFIT INFO: Inet (after scale3 abspack): min=-1088.2579 max=1265048.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.0468 max=25128.9121 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/104 6582 reflections read from tmp file 267 reflections are rejected (266 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 6 4 3 4 2 6 2 212 Initial Chi^2= 0.52951 Cycle 1, Chi^2= 1.02012 Current error model SIG(F2)^2 = 62.91*I_RAW + 11.31*I_BACK+(0.03457*)^2 Cycle 2, Chi^2= 1.01516 Current error model SIG(F2)^2 = 76.99*I_RAW + 8.02*I_BACK+(0.02851*)^2 Cycle 3, Chi^2= 1.00821 Current error model SIG(F2)^2 = 83.33*I_RAW + 6.76*I_BACK+(0.02647*)^2 Cycle 4, Chi^2= 1.00372 Current error model SIG(F2)^2 = 86.05*I_RAW + 6.27*I_BACK+(0.02580*)^2 Cycle 5, Chi^2= 1.00153 Current error model SIG(F2)^2 = 87.16*I_RAW + 6.07*I_BACK+(0.02557*)^2 Cycle 6, Chi^2= 1.00060 Current error model SIG(F2)^2 = 87.59*I_RAW + 6.00*I_BACK+(0.02548*)^2 Cycle 7, Chi^2= 1.00023 Current error model SIG(F2)^2 = 87.76*I_RAW + 5.97*I_BACK+(0.02545*)^2 Final Chi^2= 1.00023 Final error model SIG(F2)^2 = 87.76*I_RAW + 5.97*I_BACK+(0.02545*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1265049- 118276 658 381789.59 31.25 100.00 117828- 3452 658 28846.53 12.94 100.00 3450- 2013 658 2679.26 6.13 99.24 2011- 1162 658 1514.12 3.88 64.74 1162- 773 658 948.84 2.75 25.99 773- 516 658 642.34 2.38 15.50 516- 330 658 417.42 1.95 8.66 329- 151 658 241.23 1.46 3.19 151- 20 658 81.25 0.73 0.46 20- -1088 660 -136.93 -0.56 0.00 ------------------------------------------------------------------------------------ 1265049- -1088 6582 41689.65 6.29 41.77 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 658 104960.43 10.21 71.43 1.64- 1.26 658 80826.08 9.50 61.85 1.26- 1.06 658 63022.49 8.91 73.56 1.06- 0.96 658 43749.30 6.12 34.04 0.96- 0.88 658 21060.17 5.44 53.04 0.88- 0.80 658 41689.02 6.93 41.03 0.80- 0.75 658 17253.09 3.92 22.49 0.75- 0.71 658 18857.96 4.79 20.06 0.71- 0.67 658 22230.30 5.40 32.37 0.67- 0.63 660 3364.17 1.70 7.88 ------------------------------------------------------------------------------------ 6.00- 0.63 6582 41689.65 6.29 41.77 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 658 104960.43 10.21 71.43 6.00- 1.26 1316 92893.25 9.85 66.64 6.00- 1.06 1974 82936.33 9.54 68.95 6.00- 0.96 2632 73139.57 8.68 60.22 6.00- 0.88 3290 62723.69 8.03 58.78 6.00- 0.80 3948 59217.91 7.85 55.83 6.00- 0.75 4606 53222.94 7.29 51.06 6.00- 0.71 5264 48927.32 6.98 47.19 6.00- 0.67 5922 45960.98 6.80 45.54 6.00- 0.63 6582 41689.65 6.29 41.77 ------------------------------------------------------------------------------------ 6.00- 0.63 6582 41689.65 6.29 41.77 Scale applied to data: s=0.790483 (maximum obs:1265048.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.061; Rsigma 0.037: data 6582 -> merged 240 With outlier rejection... Rint 0.052; Rsigma 0.037: data 6560 -> merged 240 Rejected total: 22, method kkm 11, method Blessing 11 Completeness direct cell (a, b, c) = (10.410, 10.410, 10.410), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626634, 6.010459 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.43 - 1.59 21 21 35.52 100.00 746 1.57 - 1.20 21 21 37.00 100.00 777 1.19 - 1.02 21 21 34.95 100.00 734 1.02 - 0.91 21 21 33.71 100.00 708 0.91 - 0.84 21 21 29.86 100.00 627 0.84 - 0.78 21 21 29.29 100.00 615 0.78 - 0.74 21 21 27.71 100.00 582 0.74 - 0.71 21 21 23.62 100.00 496 0.71 - 0.68 21 21 25.76 100.00 541 0.68 - 0.65 23 23 22.00 100.00 506 --------------------------------------------------------------- 10.43 - 0.65 212 212 29.87 100.00 6332 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:59:05 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.407568 10.417910 10.405787 89.9767 89.9982 90.0056 6560 Reflections read from file xs2212a.hkl 6523 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.27 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3276 0 4329 4317 6523 N (int>3sigma) = 0 0 0 0 1454 0 1920 1884 2731 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 33.6 31.8 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.4 6.3 6.3 Lattice type: F chosen Volume: 1128.25 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.359 7.359 7.361 119.97 119.97 90.01 Niggli form: a.a = 54.148 b.b = 54.151 c.c = 54.181 b.c = -27.063 a.c = -27.056 a.b = -0.009 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.098 CUBIC F-lattice R(int) = 0.052 [ 6292] Vol = 1128.2 Cell: 10.418 10.408 10.406 90.00 90.02 89.99 Volume: 1128.25 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.037 TETRAGONAL I-lattice R(int) = 0.051 [ 5906] Vol = 564.1 Cell: 7.363 7.363 10.406 89.98 89.98 89.94 Volume: 564.12 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.024 TETRAGONAL I-lattice R(int) = 0.052 [ 5906] Vol = 564.1 Cell: 7.359 7.359 10.418 89.99 89.98 90.01 Volume: 564.12 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.089 TETRAGONAL I-lattice R(int) = 0.051 [ 5906] Vol = 564.1 Cell: 7.363 7.363 10.406 90.02 89.98 90.06 Volume: 564.12 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.017 ORTHORHOMBIC F-lattice R(int) = 0.050 [ 5853] Vol = 1128.2 Cell: 10.406 10.408 10.418 89.99 90.02 90.00 Volume: 1128.25 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.052 ORTHORHOMBIC I-lattice R(int) = 0.051 [ 5833] Vol = 564.1 Cell: 10.406 7.363 7.363 89.94 89.98 89.98 Volume: 564.12 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.024 ORTHORHOMBIC I-lattice R(int) = 0.050 [ 5833] Vol = 564.1 Cell: 7.359 7.359 10.418 90.01 90.02 90.01 Volume: 564.12 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.023 MONOCLINIC I-lattice R(int) = 0.049 [ 5306] Vol = 564.1 Cell: 7.363 10.406 7.363 89.98 90.06 90.02 Volume: 564.12 Matrix:-0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.007 MONOCLINIC I-lattice R(int) = 0.049 [ 5306] Vol = 564.1 Cell: 7.361 10.408 7.364 90.00 90.07 89.99 Volume: 564.12 Matrix: 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.007 MONOCLINIC I-lattice R(int) = 0.049 [ 5306] Vol = 564.1 Cell: 7.363 10.406 7.363 90.02 90.06 89.98 Volume: 564.12 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.021 MONOCLINIC I-lattice R(int) = 0.048 [ 5285] Vol = 564.1 Cell: 7.359 7.359 10.418 89.98 90.01 89.99 Volume: 564.12 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.016 MONOCLINIC I-lattice R(int) = 0.049 [ 5293] Vol = 564.1 Cell: 7.359 7.359 10.418 89.99 90.02 89.99 Volume: 564.12 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.016 MONOCLINIC I-lattice R(int) = 0.048 [ 5305] Vol = 564.1 Cell: 7.359 10.418 7.359 89.99 90.01 89.98 Volume: 564.12 Matrix: 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.048 MONOCLINIC I-lattice R(int) = 0.048 [ 5305] Vol = 564.1 Cell: 7.359 10.418 7.359 90.01 90.01 90.02 Volume: 564.12 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) = 0.044 [ 4243] Vol = 282.1 Cell: 7.359 7.359 7.361 119.97 119.97 90.01 Volume: 282.06 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -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 3276 0 4340 4336 6523 N (int>3sigma) = 0 0 0 0 1454 0 1938 1918 2731 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 31.9 33.1 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.4 6.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.384 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 48 48 488 1280 N I>3s 2 2 2 676 0.0 0.0 0.0 2.0 0.8 0.8 0.2 4.9 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 0.052 5832 Fd-3m 1 1 227 C N N N N 37 2284 0.053 5894 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.417910 10.407568 10.405787 89.9982 90.0233 89.9944 ZERR 5.00 0.001342 0.001344 0.000998 0.0092 0.0092 0.0105 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1151064- 126879 653 640 26 24.6 380224.11 31.20 0.048 0.064 108403- 3157 741 739 26 28.4 26891.21 12.22 0.070 0.086 2998- 1390 952 948 26 36.5 2227.26 5.55 0.130 0.184 1362- 834 830 830 26 31.9 1056.08 2.76 0.236 0.306 822- 499 805 805 26 31.0 645.68 2.30 0.305 0.410 499- 309 793 793 26 30.5 389.11 1.76 0.433 0.581 303- 140 627 626 26 24.1 227.91 1.32 0.577 1.045 138- 21 610 609 26 23.4 73.41 0.53 0.881 2.175 19- -169 571 570 32 17.8 -27.37 -0.06 0.984 4.402 ------------------------------------------------------------------------------------------- 1151064- -169 6582 6560 240 27.3 40732.34 6.24 0.052 0.070 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-1.44 961 955 26 36.7 114985.26 11.25 0.045 0.059 0.028 1.39-1.09 1003 999 26 38.4 43731.75 7.37 0.049 0.065 0.034 1.06-0.94 841 838 26 32.2 38449.76 5.70 0.047 0.062 0.036 0.92-0.84 799 798 26 30.7 41869.93 7.52 0.061 0.082 0.041 0.84-0.78 778 776 26 29.8 23962.31 4.98 0.059 0.079 0.047 0.78-0.73 691 690 27 25.6 13309.02 3.83 0.075 0.095 0.063 0.72-0.69 669 669 26 25.7 14493.29 3.95 0.078 0.092 0.067 0.68-0.66 602 600 27 22.2 14404.42 3.83 0.078 0.105 0.068 0.65-0.63 238 235 30 7.8 8321.06 2.49 0.086 0.095 0.085 ------------------------------------------------------------------------------------------------------ inf-0.63 6582 6560 240 27.3 40732.34 6.24 0.052 0.070 0.037 inf-0.65 6349 6330 211 30.0 41976.88 6.39 0.052 0.069 0.037 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-1.44 955 26 26 100.0 36.7 114985.26 68.59 0.045 0.006 1.39-1.09 999 26 26 100.0 38.4 43731.75 41.66 0.049 0.007 1.06-0.94 838 26 26 100.0 32.2 38449.76 33.30 0.047 0.007 0.92-0.84 798 26 26 100.0 30.7 41869.93 41.43 0.061 0.008 0.84-0.78 776 26 26 100.0 29.8 23962.31 25.78 0.059 0.009 0.78-0.73 690 27 27 100.0 25.6 13309.02 19.48 0.075 0.013 0.72-0.69 669 26 26 100.0 25.7 14493.29 18.89 0.078 0.014 0.68-0.66 600 27 27 100.0 22.2 14404.42 19.53 0.078 0.015 0.65-0.63 235 30 30 100.0 7.8 8321.06 6.75 0.086 0.033 -------------------------------------------------------------------------------------------- inf-0.63 6560 240 240 100.0 27.3 40732.34 34.67 0.052 0.008 inf-0.65 6330 211 211 100.0 30.0 41976.88 35.72 0.052 0.008 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066099 0.015131 0.006800 ( 0.000009 0.000009 0.000009 ) -0.016222 0.064775 0.013275 ( 0.000009 0.000009 0.000009 ) -0.003519 -0.014496 0.066512 ( 0.000007 0.000006 0.000007 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000001 0.000001 ) 0.000000 0.004635 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000001 0.004646 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066099 0.015131 0.006800 ( 0.000009 0.000009 0.000009 ) -0.016222 0.064775 0.013275 ( 0.000009 0.000009 0.000009 ) -0.003519 -0.014496 0.066512 ( 0.000007 0.000006 0.000007 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4077(13) 10.4186(14) 10.4058(10) 89.983(9) 90.001(9) 90.005(11) V = 1128.3(2) unit cell: 10.4107(3) 10.4107(3) 10.4107(3) 90.0 90.0 90.0 V = 1128.34(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.131) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.005) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.045) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.045) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.045) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) PROFFIT INFO: signal sum: min=-743.0000 max=7943242.0000 PROFFIT INFO: signal sum lp corr: min=-736.9381 max=1263717.5630 PROFFIT INFO: background sum: min=-80.0000 max=8164.0000 PROFFIT INFO: background sum sig2: min=440.0000 max=5768.0000 PROFFIT INFO: num of signal pixels: min=41 max=513 PROFFIT INFO: Inet: min=-1179.1011 max=2021948.2500 PROFFIT INFO: sig(Inet): min=52.2344 max=30724.9844 PROFFIT INFO: Inet/sig(Inet): min=-1.97 max=276.25 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 1154 4522 6838 8160 8806 10228 11110 11656 12468 13022 13164 Percent 8.8 34.4 51.9 62.0 66.9 77.7 84.4 88.5 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 6582 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 6582 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2021948- 131112 658 417401.24 77.99 100.00 130948- 4053 658 28870.91 19.38 100.00 4051- 2109 658 2900.51 7.06 97.11 2109- 1246 658 1606.68 3.95 52.74 1246- 820 658 1013.72 2.35 16.26 819- 547 658 675.77 1.73 8.36 547- 342 658 440.60 1.23 5.17 341- 157 658 247.50 0.72 0.61 157- 19 658 82.61 0.30 0.00 19- -1179 660 -138.10 -0.27 0.00 ------------------------------------------------------------------------------------ 2021948- -1179 6582 45296.33 11.44 38.01 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 658 111403.63 15.65 68.09 1.64- 1.26 658 88560.72 21.42 58.97 1.26- 1.06 658 68565.32 20.20 69.15 1.06- 0.96 658 47981.41 13.34 31.61 0.96- 0.88 658 23190.64 8.58 46.05 0.88- 0.80 658 45096.22 12.73 34.80 0.80- 0.75 658 18975.10 5.88 19.76 0.75- 0.71 658 20981.93 6.82 16.41 0.71- 0.67 658 24745.92 8.03 29.03 0.67- 0.63 660 3589.21 1.78 6.36 ------------------------------------------------------------------------------------ 6.00- 0.63 6582 45296.33 11.44 38.01 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 14:59:05 2019 Sorting 6582 observations 43 unique observations with > 7.00 F2/sig(F2) 6582 observations in 7 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 Total number of frames 661 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 16 frame = 1 scale 6582 observations in 7 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 2 45 Total number of frames 45 1591 observations > 7.00 F2/sig(F2) 1591 observations in 7 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 2 45 Total number of frames 45 Removing 'redundancy=1' reflections Average redundancy: 28.4 (Out of 1591 removed 3 = 1588, unique = 56) 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 1588 observations in 7 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 2 45 Total number of frames 45 56 unique data precomputed (should be 56) 56 unique data with 1588 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 28.4 (Out of 1588 removed 0 = 1588, unique = 56) 56 unique data precomputed (should be 56) 56 unique data with 1588 observations RMS deviation of equivalent data = 0.31432 Rint = 0.25563 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24681, wR= 0.34007 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13713, wR= 0.18990, Acormin=0.471, Acormax=1.434, Acor_av=0.996 F test: Probability=1.000, F= 3.229 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13415, wR= 0.18354, Acormin=0.477, Acormax=1.482, Acor_av=0.979 F test: Probability=0.793, F= 1.043 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12999, wR= 0.18155, Acormin=0.550, Acormax=1.546, Acor_av=1.002 F test: Probability=0.975, F= 1.106 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12481, wR= 0.17267, Acormin=0.494, Acormax=1.572, Acor_av=0.989 F test: Probability=0.938, F= 1.083 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10579, wR= 0.15365, Acormin=0.563, Acormax=1.828, Acor_av=1.036 F test: Probability=1.000, F= 1.500 Final absorption model (ne=4, no=3): Rint= 0.10579, Acormin=0.563, Acormax=1.828, Acor_av=1.036 Combined refinement in use Rint: 0.25750 There are 45 active scales (one needs to be fixed) Refinement control: frame scale #32 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 68 pars with 2346 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31432 Using Levenberg-Marquardt: 0.00010 New wR= 0.12240 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25563 with corrections 0.09030 Rint for all data: 0.25750 with corrections 0.09292 4 observations identified as outliers and rejected Cycle 2 wR= 0.11115 Using Levenberg-Marquardt: 0.00001 New wR= 0.09476 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25532 with corrections 0.06044 Rint for all data: 0.25750 with corrections 0.06604 2 observations identified as outliers and rejected Cycle 3 wR= 0.08550 Using Levenberg-Marquardt: 0.00000 New wR= 0.08001 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25456 with corrections 0.05384 Rint for all data: 0.25750 with corrections 0.05999 0 observations identified as outliers and rejected Cycle 4 wR= 0.08001 Using Levenberg-Marquardt: 0.00000 New wR= 0.07837 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25456 with corrections 0.05194 Rint for all data: 0.25750 with corrections 0.05789 1 observations identified as outliers and rejected Cycle 5 wR= 0.07386 Using Levenberg-Marquardt: 0.00000 New wR= 0.07435 Using Levenberg-Marquardt: 0.00000 New wR= 0.07435 Using Levenberg-Marquardt: 0.00000 New wR= 0.07435 Using Levenberg-Marquardt: 0.00001 New wR= 0.07435 Using Levenberg-Marquardt: 0.00010 New wR= 0.07435 Using Levenberg-Marquardt: 0.00100 New wR= 0.07435 Using Levenberg-Marquardt: 0.01000 New wR= 0.07432 Using Levenberg-Marquardt: 0.10000 New wR= 0.07410 Using Levenberg-Marquardt: 1.00000 New wR= 0.07359 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25315 with corrections 0.04944 Rint for all data: 0.25750 with corrections 0.05628 0 observations identified as outliers and rejected Final wR= 0.07359 Final frame scales: Min= 0.7068 Max= 1.2350 Final absorption correction factors: Amin= 0.3312 Amax= 1.5808 PROFFIT INFO: Inet (after scale3 abspack): min=-1139.6837 max=1265721.1250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=40.2946 max=25382.9121 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/104 6582 reflections read from tmp file 248 reflections are rejected (248 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 1 3 1 3 1 3 2 148 Initial Chi^2= 0.52427 Cycle 1, Chi^2= 1.01668 Current error model SIG(F2)^2 = 62.73*I_RAW + 12.02*I_BACK+(0.03287*)^2 Cycle 2, Chi^2= 1.01445 Current error model SIG(F2)^2 = 76.76*I_RAW + 8.51*I_BACK+(0.02762*)^2 Cycle 3, Chi^2= 1.00664 Current error model SIG(F2)^2 = 82.13*I_RAW + 7.37*I_BACK+(0.02643*)^2 Cycle 4, Chi^2= 1.00241 Current error model SIG(F2)^2 = 84.00*I_RAW + 7.01*I_BACK+(0.02618*)^2 Cycle 5, Chi^2= 1.00083 Current error model SIG(F2)^2 = 84.63*I_RAW + 6.89*I_BACK+(0.02612*)^2 Cycle 6, Chi^2= 1.00028 Current error model SIG(F2)^2 = 84.84*I_RAW + 6.85*I_BACK+(0.02610*)^2 Cycle 7, Chi^2= 1.00009 Current error model SIG(F2)^2 = 84.91*I_RAW + 6.83*I_BACK+(0.02609*)^2 Final Chi^2= 1.00009 Final error model SIG(F2)^2 = 84.91*I_RAW + 6.83*I_BACK+(0.02609*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1265721- 117722 658 380690.31 30.93 100.00 117559- 3451 658 28892.28 13.05 100.00 3447- 2023 658 2679.56 6.21 99.24 2022- 1156 658 1515.38 3.94 67.48 1155- 776 658 949.60 2.77 25.84 776- 521 658 644.16 2.39 15.65 520- 330 658 418.04 1.95 8.81 330- 151 658 241.22 1.45 3.19 150- 20 658 80.99 0.72 0.46 20- -1140 660 -137.72 -0.55 0.00 ------------------------------------------------------------------------------------ 1265721- -1140 6582 41584.70 6.28 42.05 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 658 103831.43 10.18 71.43 1.64- 1.26 658 80495.94 9.46 62.16 1.26- 1.06 658 63016.28 8.88 73.56 1.06- 0.96 658 43816.63 6.08 34.35 0.96- 0.88 658 21313.91 5.46 53.34 0.88- 0.80 658 41533.65 6.92 41.64 0.80- 0.75 658 17277.28 3.92 22.49 0.75- 0.71 658 19007.68 4.80 20.52 0.71- 0.67 658 22296.81 5.45 33.13 0.67- 0.63 660 3373.51 1.71 8.03 ------------------------------------------------------------------------------------ 6.00- 0.63 6582 41584.70 6.28 42.05 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 658 103831.43 10.18 71.43 6.00- 1.26 1316 92163.68 9.82 66.79 6.00- 1.06 1974 82447.88 9.51 69.05 6.00- 0.96 2632 72790.07 8.65 60.37 6.00- 0.88 3290 62494.84 8.01 58.97 6.00- 0.80 3948 59001.31 7.83 56.08 6.00- 0.75 4606 53040.73 7.27 51.28 6.00- 0.71 5264 48786.60 6.96 47.44 6.00- 0.67 5922 45843.29 6.79 45.85 6.00- 0.63 6582 41584.70 6.28 42.05 ------------------------------------------------------------------------------------ 6.00- 0.63 6582 41584.70 6.28 42.05 Scale applied to data: s=0.790063 (maximum obs:1265721.125,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.056; Rsigma 0.037: data 6582 -> merged 162 With outlier rejection... Rint 0.050; Rsigma 0.037: data 6564 -> merged 162 Rejected total: 18, method kkm 8, method Blessing 10 Completeness direct cell (a, b, c) = (10.411, 10.411, 10.411), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626650, 6.010616 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.43 - 1.76 14 14 42.79 100.00 599 1.74 - 1.27 14 14 46.71 100.00 654 1.26 - 1.06 14 14 53.00 100.00 742 1.05 - 0.97 14 14 46.29 100.00 648 0.95 - 0.88 14 14 48.57 100.00 680 0.87 - 0.81 14 14 43.07 100.00 603 0.80 - 0.76 14 14 45.36 100.00 635 0.76 - 0.72 14 14 37.64 100.00 527 0.72 - 0.69 14 14 41.79 100.00 585 0.69 - 0.65 19 19 34.89 100.00 663 --------------------------------------------------------------- 10.43 - 0.65 145 145 43.70 100.00 6336 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 14:59:05 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.407568 10.417910 10.405787 89.9767 89.9982 90.0056 6560 Reflections read from file xs2212a.hkl 6523 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.27 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3276 0 4329 4317 6523 N (int>3sigma) = 0 0 0 0 1454 0 1920 1884 2731 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 33.6 31.8 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.4 6.3 6.3 Lattice type: F chosen Volume: 1128.25 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -0.5000 Unitcell: 7.359 7.359 7.361 119.97 119.97 90.01 Niggli form: a.a = 54.148 b.b = 54.151 c.c = 54.181 b.c = -27.063 a.c = -27.056 a.b = -0.009 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.098 CUBIC F-lattice R(int) = 0.052 [ 6292] Vol = 1128.2 Cell: 10.418 10.408 10.406 90.00 90.02 89.99 Volume: 1128.25 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.037 TETRAGONAL I-lattice R(int) = 0.051 [ 5906] Vol = 564.1 Cell: 7.363 7.363 10.406 89.98 89.98 89.94 Volume: 564.12 Matrix: 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.024 TETRAGONAL I-lattice R(int) = 0.052 [ 5906] Vol = 564.1 Cell: 7.359 7.359 10.418 89.99 89.98 90.01 Volume: 564.12 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.089 TETRAGONAL I-lattice R(int) = 0.051 [ 5906] Vol = 564.1 Cell: 7.363 7.363 10.406 90.02 89.98 90.06 Volume: 564.12 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.017 ORTHORHOMBIC F-lattice R(int) = 0.050 [ 5853] Vol = 1128.2 Cell: 10.406 10.408 10.418 89.99 90.02 90.00 Volume: 1128.25 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.052 ORTHORHOMBIC I-lattice R(int) = 0.051 [ 5833] Vol = 564.1 Cell: 10.406 7.363 7.363 89.94 89.98 89.98 Volume: 564.12 Matrix: 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.024 ORTHORHOMBIC I-lattice R(int) = 0.050 [ 5833] Vol = 564.1 Cell: 7.359 7.359 10.418 90.01 90.02 90.01 Volume: 564.12 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.023 MONOCLINIC I-lattice R(int) = 0.049 [ 5306] Vol = 564.1 Cell: 7.363 10.406 7.363 89.98 90.06 90.02 Volume: 564.12 Matrix:-0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.007 MONOCLINIC I-lattice R(int) = 0.049 [ 5306] Vol = 564.1 Cell: 7.361 10.408 7.364 90.00 90.07 89.99 Volume: 564.12 Matrix: 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.007 MONOCLINIC I-lattice R(int) = 0.049 [ 5306] Vol = 564.1 Cell: 7.363 10.406 7.363 90.02 90.06 89.98 Volume: 564.12 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.021 MONOCLINIC I-lattice R(int) = 0.048 [ 5285] Vol = 564.1 Cell: 7.359 7.359 10.418 89.98 90.01 89.99 Volume: 564.12 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.016 MONOCLINIC I-lattice R(int) = 0.049 [ 5293] Vol = 564.1 Cell: 7.359 7.359 10.418 89.99 90.02 89.99 Volume: 564.12 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.016 MONOCLINIC I-lattice R(int) = 0.048 [ 5305] Vol = 564.1 Cell: 7.359 10.418 7.359 89.99 90.01 89.98 Volume: 564.12 Matrix: 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.048 MONOCLINIC I-lattice R(int) = 0.048 [ 5305] Vol = 564.1 Cell: 7.359 10.418 7.359 90.01 90.01 90.02 Volume: 564.12 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) = 0.044 [ 4243] Vol = 282.1 Cell: 7.359 7.359 7.361 119.97 119.97 90.01 Volume: 282.06 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 -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 3276 0 4340 4336 6523 N (int>3sigma) = 0 0 0 0 1454 0 1938 1918 2731 Mean intensity = 0.0 0.0 0.0 0.0 1.5 0.0 31.9 33.1 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.4 6.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.384 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 48 48 488 1280 N I>3s 2 2 2 676 0.0 0.0 0.0 2.0 0.8 0.8 0.2 4.9 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 0.052 5832 Fd-3m 1 1 227 C N N N N 37 2284 0.053 5894 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.417910 10.407568 10.405787 89.9982 90.0233 89.9944 ZERR 5.00 0.001342 0.001344 0.000998 0.0092 0.0092 0.0105 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1145200- 94230 798 788 27 29.2 331558.37 29.10 0.046 0.060 77438- 1797 1239 1235 27 45.7 5189.23 8.33 0.082 0.086 1647- 772 1334 1332 27 49.3 1126.12 3.00 0.226 0.300 761- 328 1291 1291 27 47.8 496.38 2.00 0.368 0.519 327- 82 934 933 27 34.6 211.75 1.19 0.613 1.168 81- -169 986 985 27 36.5 11.61 0.19 0.957 3.905 ------------------------------------------------------------------------------------------- 1145200- -169 6582 6564 162 40.5 41137.49 6.26 0.050 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-1.27 1255 1251 27 46.3 95556.58 10.20 0.044 0.057 0.029 1.26-0.97 1325 1320 27 48.9 51963.41 7.33 0.045 0.057 0.034 0.97-0.81 1293 1291 27 47.8 31969.66 6.30 0.055 0.070 0.043 0.81-0.73 1144 1142 27 42.3 11198.59 3.20 0.062 0.079 0.063 0.73-0.67 986 985 27 36.5 26108.73 5.92 0.069 0.089 0.056 0.67-0.63 579 575 27 21.3 3677.90 1.78 0.109 0.076 0.132 ------------------------------------------------------------------------------------------------------ inf-0.63 6582 6564 162 40.5 41137.49 6.26 0.050 0.063 0.037 inf-0.65 6349 6334 144 44.0 42403.30 6.41 0.050 0.063 0.037 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-1.27 1251 27 27 100.0 46.3 95556.58 66.79 0.044 0.006 1.26-0.97 1320 27 27 100.0 48.9 51963.41 48.58 0.045 0.006 0.97-0.81 1291 27 27 100.0 47.8 31969.66 43.18 0.055 0.008 0.81-0.73 1142 27 27 100.0 42.3 11198.59 19.56 0.062 0.011 0.73-0.67 985 27 27 100.0 36.5 26108.73 36.58 0.069 0.010 0.67-0.63 575 27 27 100.0 21.3 3677.90 8.49 0.109 0.029 -------------------------------------------------------------------------------------------- inf-0.63 6564 162 162 100.0 40.5 41137.49 40.62 0.050 0.008 inf-0.65 6334 144 144 100.0 44.0 42403.30 41.86 0.050 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 15:05:11 2019) ID: 3668; threads 40; handles 809; mem 515712.00 (1204692.00)kB; time: 1w 5d 1h 15m 59s MEMORY INFO: Memory PF:227.0, Ph:558.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:503.6,peak PF: 700.2, WS: 471.7, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:229.0, Ph:560.0, V:1179.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:505.4,peak PF: 700.2, WS: 473.5, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 15:05:11 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000013 0.000013 0.000013 ) -0.015931 0.064696 0.013068 ( 0.000011 0.000012 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000015 ) 10.42433 ( 0.00193 ) 10.43788 ( 0.00185 ) 10.40727 ( 0.00221 ) 89.88512 ( 0.01590 ) 89.79539 ( 0.01611 ) 90.20497 ( 0.01475 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 15:05:11 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000013 0.000013 0.000013 ) -0.015931 0.064696 0.013068 ( 0.000011 0.000012 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004645 -0.000001 -0.000008 ( 0.000002 0.000001 0.000001 ) -0.000001 0.004643 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000008 -0.000003 0.004645 ( 0.000001 0.000001 0.000002 ) unit cell: 10.4243(19) 10.4379(19) 10.407(2) 89.885(16) 89.795(16) 90.205(15) V = 1132.4(4) unit cell: 10.4082(6) 10.4082(6) 10.4082(6) 90.0 90.0 90.0 V = 1127.53(11) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.938 ( 0.170) | 0.923 ( 0.398) | 1.01- 0.88 | 22 | 0.957 ( 0.073) | 1.004 ( 0.124) | 1.180 ( 0.493) | 0.88- 0.79 | 22 | 0.985 ( 0.059) | 1.028 ( 0.140) | 1.234 ( 0.387) | 0.79- 0.70 | 22 | 0.984 ( 0.041) | 0.962 ( 0.107) | 1.276 ( 0.475) | 0.70- 0.63 | 22 | 0.943 ( 0.038) | 0.917 ( 0.081) | 1.311 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 220 | 0.933 ( 0.193) | 0.943 ( 0.158) | 1.113 ( 0.914) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.919 ( 0.072) | 0.920 ( 0.102) | 1.048 ( 0.586) | 1.19- 1.09 | 25 | 0.936 ( 0.063) | 0.971 ( 0.116) | 0.827 ( 0.253) | 1.09- 0.92 | 25 | 0.955 ( 0.078) | 0.981 ( 0.099) | 1.062 ( 0.467) | 0.92- 0.86 | 25 | 0.944 ( 0.067) | 0.942 ( 0.097) | 1.020 ( 0.391) | 0.82- 0.73 | 25 | 0.957 ( 0.050) | 0.911 ( 0.086) | 1.356 ( 0.420) | 0.73- 0.63 | 28 | 0.929 ( 0.038) | 0.881 ( 0.096) | 1.353 ( 0.467) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 253 | 0.922 ( 0.081) | 0.920 ( 0.121) | 1.063 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.156) HKL list info: 1283 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 192 peaks identified as outliers and rejected 192 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 192 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 192 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.97 | 19 | 0.842 ( 0.116) | 0.844 ( 0.171) | 0.956 ( 0.449) | 2.63- 1.84 | 19 | 0.822 ( 0.111) | 0.843 ( 0.187) | 0.847 ( 0.504) | 1.84- 1.59 | 19 | 0.842 ( 0.108) | 0.837 ( 0.164) | 0.836 ( 0.354) | 1.59- 1.36 | 19 | 0.936 ( 0.096) | 0.973 ( 0.144) | 0.805 ( 0.268) | 1.36- 1.20 | 19 | 0.950 ( 0.102) | 0.972 ( 0.160) | 0.845 ( 0.330) | 1.20- 1.01 | 19 | 0.995 ( 0.078) | 1.010 ( 0.137) | 1.101 ( 0.434) | 1.01- 0.88 | 19 | 0.998 ( 0.085) | 1.016 ( 0.121) | 1.030 ( 0.364) | 0.88- 0.79 | 19 | 1.037 ( 0.059) | 1.056 ( 0.123) | 0.938 ( 0.316) | 0.79- 0.72 | 19 | 1.031 ( 0.054) | 0.994 ( 0.144) | 1.279 ( 0.526) | 0.70- 0.63 | 21 | 0.975 ( 0.052) | 0.883 ( 0.059) | 1.164 ( 0.415) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 192 | 0.943 ( 0.117) | 0.942 ( 0.164) | 0.982 ( 0.432) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) UB - matrix: 0.065810 0.015591 0.006262 ( 0.000023 0.000019 0.000022 ) -0.016403 0.064531 0.013131 ( 0.000023 0.000020 0.000022 ) -0.002751 -0.014148 0.066421 ( 0.000026 0.000022 0.000025 ) M - matrix: 0.004608 0.000006 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004607 0.000005 ( 0.000002 0.000003 0.000002 ) 0.000014 0.000005 0.004623 ( 0.000002 0.000002 0.000003 ) unit cell: 10.450(3) 10.450(3) 10.432(4) 90.07(3) 90.17(3) 90.08(3) V = 1139.1(6) OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 1279 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 189 peaks identified as outliers and rejected 189 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 189 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 189 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 3.00 | 19 | 0.846 ( 0.114) | 0.847 ( 0.168) | 0.873 ( 0.501) | 2.99- 2.00 | 19 | 0.802 ( 0.108) | 0.800 ( 0.186) | 0.843 ( 0.452) | 1.84- 1.59 | 19 | 0.842 ( 0.097) | 0.828 ( 0.155) | 0.880 ( 0.351) | 1.59- 1.36 | 19 | 0.948 ( 0.083) | 0.983 ( 0.140) | 0.851 ( 0.258) | 1.36- 1.19 | 19 | 0.948 ( 0.091) | 0.960 ( 0.152) | 0.770 ( 0.212) | 1.19- 1.00 | 19 | 1.009 ( 0.064) | 1.035 ( 0.123) | 1.078 ( 0.369) | 1.00- 0.88 | 19 | 1.020 ( 0.083) | 1.045 ( 0.136) | 1.050 ( 0.370) | 0.88- 0.78 | 19 | 1.033 ( 0.056) | 1.041 ( 0.111) | 0.945 ( 0.325) | 0.78- 0.69 | 19 | 1.025 ( 0.054) | 0.983 ( 0.157) | 1.279 ( 0.530) | 0.69- 0.63 | 18 | 0.969 ( 0.052) | 0.877 ( 0.057) | 1.147 ( 0.364) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 189 | 0.944 ( 0.116) | 0.940 ( 0.168) | 0.971 ( 0.414) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 UB - matrix: 0.066110 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) UB - matrix: 0.066109 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) 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= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 100 peaks identified as outliers and rejected 100 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 100 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 100 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 2.37 | 10 | 0.824 ( 0.107) | 0.789 ( 0.168) | 0.948 ( 0.526) | 2.13- 1.65 | 10 | 0.887 ( 0.099) | 0.902 ( 0.146) | 0.800 ( 0.370) | 1.64- 1.46 | 10 | 0.917 ( 0.142) | 0.896 ( 0.234) | 0.948 ( 0.416) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.161) | 1.038 ( 0.459) | 1.23- 1.11 | 10 | 1.014 ( 0.089) | 1.022 ( 0.172) | 1.004 ( 0.500) | 1.11- 1.00 | 10 | 0.988 ( 0.107) | 1.011 ( 0.206) | 0.971 ( 0.392) | 1.00- 0.89 | 10 | 1.016 ( 0.106) | 1.093 ( 0.173) | 0.829 ( 0.141) | 0.89- 0.86 | 10 | 0.995 ( 0.094) | 1.038 ( 0.093) | 1.245 ( 0.487) | 0.82- 0.73 | 10 | 1.072 ( 0.046) | 1.130 ( 0.142) | 0.868 ( 0.108) | 0.72- 0.64 | 10 | 1.031 ( 0.064) | 1.069 ( 0.171) | 1.233 ( 0.765) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 0.64 | 100 | 0.972 ( 0.121) | 0.995 ( 0.197) | 0.988 ( 0.476) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) UB - matrix: 0.065966 0.015448 0.005965 ( 0.000053 0.000028 0.000028 ) -0.016426 0.064502 0.013369 ( 0.000054 0.000029 0.000028 ) -0.002418 -0.014553 0.066425 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004627 -0.000005 0.000013 ( 0.000007 0.000004 0.000003 ) -0.000005 0.004611 -0.000012 ( 0.000004 0.000004 0.000002 ) 0.000013 -0.000012 0.004627 ( 0.000003 0.000002 0.000002 ) unit cell: 10.427(8) 10.446(5) 10.428(3) 89.85(3) 90.16(4) 89.93(5) V = 1136(1) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) 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! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 101 peaks identified as outliers and rejected 101 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 101 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 101 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.38 | 10 | 0.825 ( 0.107) | 0.790 ( 0.169) | 1.019 ( 0.527) | 2.13- 1.64 | 10 | 0.860 ( 0.122) | 0.859 ( 0.190) | 0.860 ( 0.389) | 1.64- 1.46 | 10 | 0.944 ( 0.113) | 0.943 ( 0.190) | 0.940 ( 0.402) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.160) | 1.023 ( 0.449) | 1.23- 1.11 | 10 | 1.002 ( 0.107) | 0.995 ( 0.210) | 0.997 ( 0.506) | 1.09- 1.00 | 10 | 1.034 ( 0.082) | 1.115 ( 0.140) | 0.886 ( 0.284) | 0.97- 0.88 | 10 | 0.989 ( 0.091) | 1.159 ( 0.229) | 0.740 ( 0.286) | 0.88- 0.86 | 10 | 1.009 ( 0.084) | 1.059 ( 0.096) | 1.119 ( 0.453) | 0.82- 0.73 | 10 | 1.071 ( 0.046) | 1.128 ( 0.142) | 0.868 ( 0.110) | 0.72- 0.63 | 11 | 1.023 ( 0.066) | 1.042 ( 0.168) | 1.108 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.63 | 101 | 0.974 ( 0.119) | 1.009 ( 0.206) | 0.958 ( 0.416) | 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_8_1.rpb PROFFITPEAK info: 95 peaks in the peak location table UB fit with 32 obs out of 51 (total:51,skipped:0) (62.75%) UB - matrix: 0.065858 0.015217 0.006516 ( 0.000265 0.000197 0.000087 ) -0.016736 0.064800 0.013333 ( 0.000193 0.000143 0.000063 ) -0.003434 -0.014374 0.066617 ( 0.000290 0.000216 0.000095 ) M - matrix: 0.004629 -0.000033 -0.000023 ( 0.000036 0.000019 0.000020 ) -0.000033 0.004637 0.000006 ( 0.000019 0.000020 0.000015 ) -0.000023 0.000006 0.004658 ( 0.000020 0.000015 0.000013 ) unit cell: 10.43(4) 10.42(2) 10.393(17) 90.07(19) 89.7(2) 89.6(2) V = 1129(5) UB fit with 32 obs out of 51 (total:51,skipped:0) (62.75%) UB - matrix: 0.065858 0.015217 0.006516 ( 0.000265 0.000197 0.000087 ) -0.016736 0.064800 0.013333 ( 0.000193 0.000143 0.000063 ) -0.003434 -0.014374 0.066617 ( 0.000290 0.000216 0.000095 ) M - matrix: 0.004629 -0.000033 -0.000023 ( 0.000036 0.000019 0.000020 ) -0.000033 0.004637 0.000006 ( 0.000019 0.000020 0.000015 ) -0.000023 0.000006 0.004658 ( 0.000020 0.000015 0.000013 ) unit cell: 10.43(4) 10.42(2) 10.393(17) 90.07(19) 89.7(2) 89.6(2) V = 1129(5) OTKP changes: 21 1 1 1 OTKP changes: 21 1 1 1 OTKP changes: 21 1 1 1 No constraint UB - matrix: 0.066012 0.015307 0.006038 ( 0.000173 0.000118 0.000062 ) -0.016531 0.064783 0.013289 ( 0.000127 0.000087 0.000045 ) -0.002549 -0.014420 0.066310 ( 0.000096 0.000066 0.000034 ) M - matrix: 0.004637 -0.000024 0.000010 ( 0.000023 0.000012 0.000008 ) -0.000024 0.004639 -0.000003 ( 0.000012 0.000012 0.000006 ) 0.000010 -0.000003 0.004610 ( 0.000008 0.000006 0.000005 ) Constraint UB - matrix: 0.066012 0.015307 0.006038 ( 0.000173 0.000118 0.000062 ) -0.016531 0.064783 0.013289 ( 0.000127 0.000087 0.000045 ) -0.002549 -0.014420 0.066310 ( 0.000096 0.000066 0.000034 ) M - matrix: 0.004618 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004618 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004618 ( 0.000000 0.000000 0.000002 ) UB fit with 51 obs out of 51 (total:51,skipped:0) (100.00%) unit cell: 10.42(2) 10.414(14) 10.447(6) 89.96(7) 90.12(10) 89.71(15) V = 1133(3) unit cell: 10.425(2) 10.425(2) 10.425(2) 90.0 90.0 90.0 V = 1133.2(4) UB fit with 51 obs out of 51 (total:51,skipped:0) (100.00%) UB - matrix: 0.066012 0.015307 0.006038 ( 0.000173 0.000118 0.000062 ) -0.016531 0.064783 0.013289 ( 0.000127 0.000087 0.000045 ) -0.002549 -0.014420 0.066310 ( 0.000096 0.000066 0.000034 ) M - matrix: 0.004637 -0.000024 0.000010 ( 0.000023 0.000012 0.000008 ) -0.000024 0.004639 -0.000003 ( 0.000012 0.000012 0.000006 ) 0.000010 -0.000003 0.004610 ( 0.000008 0.000006 0.000005 ) unit cell: 10.42(2) 10.414(14) 10.447(6) 89.96(7) 90.12(10) 89.71(15) V = 1133(3) OTKP changes: 21 1 1 1 OTKP changes: 21 1 1 1 OTKP changes: 21 1 1 1 No constraint UB - matrix: 0.066016 0.015310 0.006026 ( 0.000173 0.000119 0.000062 ) -0.016532 0.064775 0.013301 ( 0.000128 0.000087 0.000046 ) -0.002552 -0.014390 0.066336 ( 0.000092 0.000063 0.000033 ) M - matrix: 0.004638 -0.000023 0.000009 ( 0.000023 0.000012 0.000008 ) -0.000023 0.004637 -0.000001 ( 0.000012 0.000012 0.000005 ) 0.000009 -0.000001 0.004614 ( 0.000008 0.000005 0.000005 ) Constraint UB - matrix: 0.066016 0.015310 0.006026 ( 0.000173 0.000119 0.000062 ) -0.016532 0.064775 0.013301 ( 0.000128 0.000087 0.000046 ) -0.002552 -0.014390 0.066336 ( 0.000092 0.000063 0.000033 ) M - matrix: 0.004619 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004619 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004619 ( 0.000000 0.000000 0.000002 ) UB fit with 51 obs out of 51 (total:51,skipped:0) (100.00%) unit cell: 10.42(2) 10.416(14) 10.443(6) 89.99(7) 90.11(10) 89.71(15) V = 1133(3) unit cell: 10.425(2) 10.425(2) 10.425(2) 90.0 90.0 90.0 V = 1132.9(4) 51 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_8" Run 8 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.156) HKL list info: 461 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 51 obs out of 51 (total:51,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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_1.rpb 0 of 40 peaks identified as outliers and rejected 40 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" 40 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8.tabbin file 40 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.15- 2.12 | 4 | 0.836 ( 0.078) | 0.822 ( 0.141) | 0.869 ( 0.327) | 2.12- 1.76 | 4 | 0.848 ( 0.124) | 0.868 ( 0.190) | 0.548 ( 0.123) | 1.75- 1.58 | 4 | 0.865 ( 0.142) | 0.823 ( 0.231) | 1.021 ( 0.572) | 1.51- 1.23 | 4 | 1.033 ( 0.028) | 1.116 ( 0.109) | 0.575 ( 0.208) | 1.23- 1.15 | 4 | 0.962 ( 0.108) | 0.951 ( 0.201) | 1.061 ( 0.488) | 1.12- 1.00 | 4 | 1.024 ( 0.046) | 1.061 ( 0.097) | 1.206 ( 0.491) | 1.00- 0.87 | 4 | 1.005 ( 0.057) | 0.996 ( 0.098) | 1.052 ( 0.199) | 0.82- 0.79 | 4 | 1.060 ( 0.017) | 1.063 ( 0.085) | 0.813 ( 0.102) | 0.79- 0.70 | 4 | 1.023 ( 0.062) | 1.067 ( 0.170) | 1.016 ( 0.214) | 0.70- 0.68 | 4 | 1.006 ( 0.078) | 0.871 ( 0.039) | 1.166 ( 0.566) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.15- 0.68 | 40 | 0.966 ( 0.116) | 0.964 ( 0.182) | 0.933 ( 0.431) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" UB fit with 40 obs out of 40 (total:40,skipped:0) (100.00%) UB - matrix: 0.065832 0.015532 0.005879 ( 0.000134 0.000089 0.000050 ) -0.016532 0.064602 0.013211 ( 0.000096 0.000064 0.000035 ) -0.002635 -0.014289 0.066449 ( 0.000063 0.000042 0.000023 ) M - matrix: 0.004614 -0.000008 -0.000007 ( 0.000018 0.000009 0.000006 ) -0.000008 0.004619 -0.000005 ( 0.000009 0.000009 0.000004 ) -0.000007 -0.000005 0.004625 ( 0.000006 0.000004 0.000003 ) unit cell: 10.44(2) 10.437(10) 10.430(4) 89.94(5) 89.92(7) 89.90(11) V = 1137(2) OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 No constraint UB - matrix: 0.065866 0.015597 0.005971 ( 0.000085 0.000056 0.000031 ) -0.016426 0.064738 0.013281 ( 0.000079 0.000053 0.000029 ) -0.002607 -0.014319 0.066430 ( 0.000055 0.000036 0.000020 ) M - matrix: 0.004615 0.000001 0.000002 ( 0.000012 0.000007 0.000004 ) 0.000001 0.004639 0.000002 ( 0.000007 0.000007 0.000003 ) 0.000002 0.000002 0.004625 ( 0.000004 0.000003 0.000003 ) Constraint UB - matrix: 0.065866 0.015597 0.005971 ( 0.000085 0.000056 0.000031 ) -0.016426 0.064738 0.013281 ( 0.000079 0.000053 0.000029 ) -0.002607 -0.014319 0.066430 ( 0.000055 0.000036 0.000020 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 40 obs out of 40 (total:40,skipped:0) (100.00%) unit cell: 10.441(13) 10.414(8) 10.430(4) 90.02(4) 90.02(5) 90.02(8) V = 1134(2) unit cell: 10.4282(15) 10.4282(15) 10.4282(15) 90.0 90.0 90.0 V = 1134.0(3) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.156) HKL list info: 463 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 40 obs out of 40 (total:40,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_1.rpb 1 of 42 peaks identified as outliers and rejected 41 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" 41 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8.tabbin file 41 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.15- 2.12 | 4 | 0.786 ( 0.073) | 0.741 ( 0.126) | 1.001 ( 0.758) | 2.11- 1.76 | 4 | 0.842 ( 0.131) | 0.830 ( 0.213) | 0.682 ( 0.216) | 1.75- 1.50 | 4 | 0.944 ( 0.125) | 0.980 ( 0.191) | 0.658 ( 0.184) | 1.46- 1.23 | 4 | 0.975 ( 0.062) | 0.979 ( 0.157) | 0.570 ( 0.223) | 1.23- 1.15 | 4 | 0.978 ( 0.082) | 0.997 ( 0.125) | 1.000 ( 0.505) | 1.11- 1.00 | 4 | 1.029 ( 0.046) | 1.078 ( 0.082) | 1.053 ( 0.187) | 1.00- 0.87 | 4 | 1.005 ( 0.056) | 0.973 ( 0.099) | 1.221 ( 0.483) | 0.82- 0.79 | 4 | 1.059 ( 0.018) | 1.068 ( 0.093) | 0.811 ( 0.101) | 0.78- 0.69 | 4 | 1.023 ( 0.062) | 1.077 ( 0.179) | 1.003 ( 0.207) | 0.69- 0.63 | 5 | 0.993 ( 0.077) | 0.880 ( 0.041) | 1.364 ( 0.537) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.15- 0.63 | 41 | 0.964 ( 0.114) | 0.958 ( 0.174) | 0.947 ( 0.470) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 154 | 0.994 ( 0.042) | 1.042 ( 0.071) | 1.109 ( 0.488) | 10.4-15.2 | 154 | 0.997 ( 0.049) | 1.053 ( 0.071) | 1.093 ( 0.502) | 15.2-19.4 | 154 | 0.996 ( 0.173) | 1.037 ( 0.102) | 1.123 ( 0.924) | 19.4-23.7 | 154 | 0.972 ( 0.066) | 1.011 ( 0.085) | 0.947 ( 0.411) | 23.7-27.7 | 154 | 0.975 ( 0.070) | 1.019 ( 0.118) | 0.950 ( 0.446) | 27.7-32.8 | 154 | 0.952 ( 0.086) | 0.969 ( 0.119) | 0.938 ( 0.428) | 32.8-36.4 | 154 | 0.918 ( 0.153) | 0.904 ( 0.149) | 1.045 ( 0.640) | 36.5-39.0 | 154 | 0.895 ( 0.108) | 0.884 ( 0.240) | 1.031 ( 0.482) | 39.0-42.0 | 154 | 0.894 ( 0.110) | 0.846 ( 0.160) | 0.984 ( 0.444) | 42.0-50.2 | 150 | 0.870 ( 0.127) | 0.793 ( 0.148) | 0.926 ( 0.426) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.2 | 1536 | 0.946 ( 0.116) | 0.956 ( 0.161) | 1.015 ( 0.545) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.14 e2 dimension: a=-0.0068 b=1.24 e3 dimension: a=-0.0004 b=1.12 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_8" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 5011 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 15:05:32 2019 PROFFITMAIN - Started at Wed Aug 21 15:05:32 2019 OTKP changes: 1185 2 7 8 OTKP changes: 1185 2 7 8 OTKP changes: 1185 2 7 8 No constraint UB - matrix: 0.066141 0.015136 0.006681 ( 0.000012 0.000013 0.000013 ) -0.016254 0.064850 0.013214 ( 0.000011 0.000012 0.000012 ) -0.003539 -0.014466 0.066512 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004651 -0.000002 -0.000008 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004644 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000008 -0.000004 0.004643 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066141 0.015136 0.006681 ( 0.000012 0.000013 0.000013 ) -0.016254 0.064850 0.013214 ( 0.000011 0.000012 0.000012 ) -0.003539 -0.014466 0.066512 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 1235 obs out of 1536 (total:1536,skipped:0) (80.40%) unit cell: 10.4003(18) 10.4086(19) 10.409(2) 89.949(16) 89.898(16) 89.978(14) V = 1126.8(4) unit cell: 10.4061(6) 10.4061(6) 10.4061(6) 90.0 90.0 90.0 V = 1126.84(12) *** 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 187 obs out of 220 (total:220,skipped:0) (85.00%) UB - matrix: 0.066500 0.011702 0.008960 ( 0.000032 0.000043 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000030 0.000040 0.000034 ) -0.006052 -0.013931 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.60(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004603 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 220 (total:220,skipped:0) (85.91%) unit cell: 10.406(5) 10.502(6) 10.456(6) 90.61(5) 90.19(4) 89.64(4) V = 1143(1) unit cell: 10.4543(19) 10.4543(19) 10.4543(19) 90.0 90.0 90.0 V = 1142.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 220 (total:220,skipped:0) (92.27%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004644 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 220 (total:220,skipped:0) (93.64%) unit cell: 10.409(4) 10.492(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1140.0(9) unit cell: 10.4466(13) 10.4466(13) 10.4466(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.066337 0.014190 0.006778 ( 0.000027 0.000035 0.000035 ) -0.015583 0.064702 0.012861 ( 0.000017 0.000023 0.000023 ) -0.004075 -0.014194 0.066900 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.2(7) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 No constraint UB - matrix: 0.066345 0.014190 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015580 0.064698 0.012867 ( 0.000017 0.000023 0.000023 ) -0.004086 -0.014196 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066345 0.014190 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015580 0.064698 0.012867 ( 0.000017 0.000023 0.000023 ) -0.004086 -0.014196 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.389(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.003) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066345 0.014190 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015580 0.064698 0.012867 ( 0.000017 0.000023 0.000023 ) -0.004086 -0.014196 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066345 0.014190 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015580 0.064698 0.012867 ( 0.000017 0.000023 0.000023 ) -0.004086 -0.014196 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.389(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068247 -0.000106 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000025 0.067887 -0.000161 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000005 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004658 -0.000006 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000006 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068247 -0.000106 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000025 0.067887 -0.000161 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000005 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.393(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4049(5) 10.4049(5) 10.4049(5) 90.0 90.0 90.0 V = 1126.44(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065883 0.015205 0.006808 ( 0.000019 0.000013 0.000019 ) -0.016068 0.064785 0.013231 ( 0.000017 0.000012 0.000016 ) -0.003637 -0.014505 0.066499 ( 0.000021 0.000015 0.000021 ) M - matrix: 0.004612 0.000014 -0.000006 ( 0.000003 0.000001 0.000002 ) 0.000014 0.004639 -0.000004 ( 0.000001 0.000002 0.000002 ) -0.000006 -0.000004 0.004644 ( 0.000002 0.000002 0.000003 ) unit cell: 10.444(3) 10.414(2) 10.409(3) 89.952(19) 89.93(2) 90.168(19) V = 1132.2(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065932 0.015224 0.006785 ( 0.000020 0.000013 0.000019 ) -0.016120 0.064843 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003639 -0.014463 0.066572 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004620 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004653 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065932 0.015224 0.006785 ( 0.000020 0.000013 0.000019 ) -0.016120 0.064843 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003639 -0.014463 0.066572 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4066(19) 10.398(3) 89.997(18) 89.89(2) 90.137(18) V = 1129.2(5) unit cell: 10.4133(5) 10.4133(5) 10.4133(5) 90.0 90.0 90.0 V = 1129.17(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.037) HKL list info: 1275 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065932 0.015224 0.006785 ( 0.000020 0.000013 0.000019 ) -0.016120 0.064843 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003639 -0.014463 0.066572 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004620 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004653 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065932 0.015224 0.006785 ( 0.000020 0.000013 0.000019 ) -0.016120 0.064843 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003639 -0.014463 0.066572 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4066(19) 10.398(3) 89.997(18) 89.89(2) 90.137(18) V = 1129.2(5) unit cell: 10.4133(5) 10.4133(5) 10.4133(5) 90.0 90.0 90.0 V = 1129.17(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065932 0.015224 0.006785 ( 0.000020 0.000013 0.000019 ) -0.016120 0.064843 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003639 -0.014463 0.066572 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004620 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004653 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065932 0.015224 0.006785 ( 0.000020 0.000013 0.000019 ) -0.016120 0.064843 0.013252 ( 0.000016 0.000011 0.000016 ) -0.003639 -0.014463 0.066572 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4066(19) 10.398(3) 89.997(18) 89.89(2) 90.137(18) V = 1129.2(5) unit cell: 10.4133(5) 10.4133(5) 10.4133(5) 90.0 90.0 90.0 V = 1129.17(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066117 0.015252 0.006582 ( 0.000015 0.000020 0.000017 ) -0.016341 0.064736 0.012926 ( 0.000012 0.000016 0.000013 ) -0.003352 -0.014201 0.066518 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004650 -0.000002 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000002 0.004625 -0.000007 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000007 0.004635 ( 0.000001 0.000001 0.000002 ) unit cell: 10.402(2) 10.430(2) 10.4185(19) 89.907(16) 90.012(17) 89.977(19) V = 1130.3(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066150 0.015268 0.006526 ( 0.000013 0.000018 0.000015 ) -0.016366 0.064786 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003345 -0.014170 0.066608 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004655 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004631 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004647 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066150 0.015268 0.006526 ( 0.000013 0.000018 0.000015 ) -0.016366 0.064786 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003345 -0.014170 0.066608 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.396(2) 10.423(2) 10.4048(18) 89.945(16) 89.960(15) 89.964(18) V = 1127.5(4) unit cell: 10.4080(5) 10.4080(5) 10.4080(5) 90.0 90.0 90.0 V = 1127.46(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.037) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066150 0.015268 0.006526 ( 0.000013 0.000018 0.000015 ) -0.016366 0.064786 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003345 -0.014170 0.066608 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004655 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004631 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004647 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066150 0.015268 0.006526 ( 0.000013 0.000018 0.000015 ) -0.016366 0.064786 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003345 -0.014170 0.066608 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.396(2) 10.423(2) 10.4048(18) 89.945(16) 89.960(15) 89.964(18) V = 1127.5(4) unit cell: 10.4080(5) 10.4080(5) 10.4080(5) 90.0 90.0 90.0 V = 1127.46(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068211 -0.000039 -0.000036 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068067 -0.000053 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068172 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004653 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004633 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004647 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068211 -0.000039 -0.000036 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068067 -0.000053 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068172 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.3986(16) 10.421(3) 10.4046(15) 89.964(16) 89.976(13) 89.968(17) V = 1127.4(4) unit cell: 10.4079(5) 10.4079(5) 10.4079(5) 90.0 90.0 90.0 V = 1127.43(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 264 obs out of 271 (total:271,skipped:0) (97.42%) UB - matrix: 0.065971 0.015330 0.006324 ( 0.000016 0.000012 0.000013 ) -0.016380 0.064793 0.013407 ( 0.000020 0.000015 0.000015 ) -0.002927 -0.014577 0.066484 ( 0.000020 0.000015 0.000015 ) M - matrix: 0.004629 -0.000007 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000007 0.004646 -0.000003 ( 0.000002 0.000002 0.000001 ) 0.000003 -0.000003 0.004640 ( 0.000002 0.000001 0.000002 ) unit cell: 10.425(2) 10.407(2) 10.413(2) 89.957(18) 90.04(2) 89.910(19) V = 1129.7(4) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.066046 0.015386 0.006332 ( 0.000016 0.000012 0.000013 ) -0.016394 0.064844 0.013378 ( 0.000018 0.000013 0.000014 ) -0.002876 -0.014635 0.066560 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004639 -0.000005 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004656 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066046 0.015386 0.006332 ( 0.000016 0.000012 0.000013 ) -0.016394 0.064844 0.013378 ( 0.000018 0.000013 0.000014 ) -0.002876 -0.014635 0.066560 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.414(2) 10.395(2) 10.4025(18) 89.887(15) 90.092(17) 89.941(18) V = 1126.1(4) unit cell: 10.4039(5) 10.4039(5) 10.4039(5) 90.0 90.0 90.0 V = 1126.13(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.037) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066046 0.015386 0.006332 ( 0.000016 0.000012 0.000013 ) -0.016394 0.064844 0.013378 ( 0.000018 0.000013 0.000014 ) -0.002876 -0.014635 0.066560 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004639 -0.000005 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004656 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066046 0.015386 0.006332 ( 0.000016 0.000012 0.000013 ) -0.016394 0.064844 0.013378 ( 0.000018 0.000013 0.000014 ) -0.002876 -0.014635 0.066560 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.414(2) 10.395(2) 10.4025(18) 89.887(15) 90.092(17) 89.941(18) V = 1126.1(4) unit cell: 10.4039(5) 10.4039(5) 10.4039(5) 90.0 90.0 90.0 V = 1126.13(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068116 -0.000094 0.000071 ( 0.000017 0.000013 0.000014 ) 0.000059 0.068201 -0.000091 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068178 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004651 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068116 -0.000094 0.000071 ( 0.000017 0.000013 0.000014 ) 0.000059 0.068201 -0.000091 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068178 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.413(3) 10.4001(16) 10.4036(18) 89.931(13) 90.044(17) 89.971(16) V = 1126.7(4) unit cell: 10.4056(5) 10.4056(5) 10.4056(5) 90.0 90.0 90.0 V = 1126.67(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 163 obs out of 189 (total:189,skipped:0) (86.24%) UB - matrix: 0.066089 0.015503 0.006319 ( 0.000027 0.000024 0.000027 ) -0.016487 0.064861 0.013040 ( 0.000028 0.000025 0.000028 ) -0.003261 -0.014176 0.066499 ( 0.000049 0.000043 0.000048 ) M - matrix: 0.004650 0.000001 -0.000014 ( 0.000004 0.000003 0.000004 ) 0.000001 0.004648 0.000001 ( 0.000003 0.000004 0.000004 ) -0.000014 0.000001 0.004632 ( 0.000004 0.000004 0.000006 ) unit cell: 10.402(4) 10.404(4) 10.422(7) 90.01(4) 89.82(5) 90.02(3) V = 1128(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 No constraint UB - matrix: 0.066038 0.015581 0.006345 ( 0.000018 0.000015 0.000018 ) -0.016420 0.064686 0.013081 ( 0.000023 0.000019 0.000022 ) -0.002866 -0.014365 0.066606 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004639 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066038 0.015581 0.006345 ( 0.000018 0.000015 0.000018 ) -0.016420 0.064686 0.013081 ( 0.000023 0.000019 0.000022 ) -0.002866 -0.014365 0.066606 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 189 obs out of 189 (total:189,skipped:0) (100.00%) unit cell: 10.414(3) 10.420(3) 10.404(2) 89.85(2) 90.165(19) 90.10(2) V = 1129.1(5) unit cell: 10.4130(7) 10.4130(7) 10.4130(7) 90.0 90.0 90.0 V = 1129.07(13) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.040) HKL list info: 1266 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066038 0.015581 0.006345 ( 0.000018 0.000015 0.000018 ) -0.016420 0.064686 0.013081 ( 0.000023 0.000019 0.000022 ) -0.002866 -0.014365 0.066606 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004639 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066038 0.015581 0.006345 ( 0.000018 0.000015 0.000018 ) -0.016420 0.064686 0.013081 ( 0.000023 0.000019 0.000022 ) -0.002866 -0.014365 0.066606 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 189 obs out of 189 (total:189,skipped:0) (100.00%) unit cell: 10.414(3) 10.420(3) 10.404(2) 89.85(2) 90.165(19) 90.10(2) V = 1129.1(5) unit cell: 10.4130(7) 10.4130(7) 10.4130(7) 90.0 90.0 90.0 V = 1129.07(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 189 obs out of 189 (total:189,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: 0.068135 0.000080 0.000193 ( 0.000019 0.000016 0.000019 ) -0.000013 0.068076 -0.000159 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068169 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000005 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000005 0.004634 -0.000011 ( 0.000002 0.000002 0.000002 ) 0.000013 -0.000011 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.068135 0.000080 0.000193 ( 0.000019 0.000016 0.000019 ) -0.000013 0.068076 -0.000159 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068169 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 189 obs out of 189 (total:189,skipped:0) (100.00%) unit cell: 10.410(3) 10.419(3) 10.4050(18) 89.867(19) 90.160(19) 90.06(2) V = 1128.6(5) unit cell: 10.4115(7) 10.4115(7) 10.4115(7) 90.0 90.0 90.0 V = 1128.60(12) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.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= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) UB - matrix: 0.066050 0.015406 0.005978 ( 0.000054 0.000029 0.000029 ) -0.016526 0.064607 0.013496 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014551 0.066437 ( 0.000034 0.000018 0.000018 ) M - matrix: 0.004641 -0.000015 0.000013 ( 0.000007 0.000003 0.000003 ) -0.000015 0.004623 -0.000003 ( 0.000003 0.000002 0.000002 ) 0.000013 -0.000003 0.004632 ( 0.000003 0.000002 0.000002 ) unit cell: 10.411(8) 10.432(3) 10.422(3) 89.97(2) 90.15(4) 89.81(4) V = 1132.0(10) OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 No constraint UB - matrix: 0.066056 0.015404 0.005976 ( 0.000054 0.000029 0.000029 ) -0.016530 0.064613 0.013504 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014547 0.066441 ( 0.000035 0.000019 0.000018 ) M - matrix: 0.004642 -0.000016 0.000012 ( 0.000007 0.000003 0.000003 ) -0.000016 0.004624 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000012 -0.000002 0.004632 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066056 0.015404 0.005976 ( 0.000054 0.000029 0.000029 ) -0.016530 0.064613 0.013504 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014547 0.066441 ( 0.000035 0.000019 0.000018 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.410(8) 10.431(3) 10.421(3) 89.98(2) 90.15(4) 89.81(4) V = 1131.7(10) unit cell: 10.4209(11) 10.4209(11) 10.4209(11) 90.0 90.0 90.0 V = 1131.7(2) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 674 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066056 0.015404 0.005976 ( 0.000054 0.000029 0.000029 ) -0.016530 0.064613 0.013504 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014547 0.066441 ( 0.000035 0.000019 0.000018 ) M - matrix: 0.004642 -0.000016 0.000012 ( 0.000007 0.000003 0.000003 ) -0.000016 0.004624 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000012 -0.000002 0.004632 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066056 0.015404 0.005976 ( 0.000054 0.000029 0.000029 ) -0.016530 0.064613 0.013504 ( 0.000030 0.000016 0.000016 ) -0.002397 -0.014547 0.066441 ( 0.000035 0.000019 0.000018 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.410(8) 10.431(3) 10.421(3) 89.98(2) 90.15(4) 89.81(4) V = 1131.7(10) unit cell: 10.4209(11) 10.4209(11) 10.4209(11) 90.0 90.0 90.0 V = 1131.7(2) 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 7) ******* No constraint UB - matrix: 0.068141 -0.000220 0.000186 ( 0.000054 0.000029 0.000028 ) -0.000007 0.067997 -0.000026 ( 0.000030 0.000016 0.000016 ) 0.000000 -0.000002 0.068061 ( 0.000035 0.000019 0.000019 ) M - matrix: 0.004643 -0.000015 0.000013 ( 0.000007 0.000003 0.000003 ) -0.000015 0.004624 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000013 -0.000002 0.004632 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.068141 -0.000220 0.000186 ( 0.000054 0.000029 0.000028 ) -0.000007 0.067997 -0.000026 ( 0.000030 0.000016 0.000016 ) 0.000000 -0.000002 0.068061 ( 0.000035 0.000019 0.000019 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.409(8) 10.431(2) 10.422(3) 89.98(2) 90.16(4) 89.81(3) V = 1131.6(10) unit cell: 10.4207(11) 10.4207(11) 10.4207(11) 90.0 90.0 90.0 V = 1131.6(2) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 56.89 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb *** 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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_proffitpeak_8" UB fit with 36 obs out of 41 (total:41,skipped:0) (87.80%) UB - matrix: 0.065692 0.015612 0.006102 ( 0.000171 0.000113 0.000062 ) -0.016402 0.064683 0.013296 ( 0.000101 0.000067 0.000036 ) -0.002886 -0.014142 0.066558 ( 0.000209 0.000138 0.000075 ) M - matrix: 0.004593 0.000005 -0.000009 ( 0.000023 0.000011 0.000015 ) 0.000005 0.004628 0.000014 ( 0.000011 0.000010 0.000010 ) -0.000009 0.000014 0.004644 ( 0.000015 0.000010 0.000010 ) unit cell: 10.47(2) 10.427(12) 10.408(13) 90.17(13) 89.88(18) 90.07(13) V = 1136(3) OTKP changes: 41 1 1 1 OTKP changes: 41 1 1 1 OTKP changes: 41 1 1 1 No constraint UB - matrix: 0.066076 0.015476 0.005970 ( 0.000100 0.000063 0.000035 ) -0.016423 0.064858 0.013326 ( 0.000084 0.000053 0.000030 ) -0.002601 -0.014364 0.066526 ( 0.000054 0.000034 0.000019 ) M - matrix: 0.004642 -0.000005 0.000003 ( 0.000013 0.000007 0.000004 ) -0.000005 0.004652 0.000001 ( 0.000007 0.000007 0.000003 ) 0.000003 0.000001 0.004639 ( 0.000004 0.000003 0.000003 ) Constraint UB - matrix: 0.066076 0.015476 0.005970 ( 0.000100 0.000063 0.000035 ) -0.016423 0.064858 0.013326 ( 0.000084 0.000053 0.000030 ) -0.002601 -0.014364 0.066526 ( 0.000054 0.000034 0.000019 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 41 obs out of 41 (total:41,skipped:0) (100.00%) unit cell: 10.410(15) 10.399(8) 10.414(3) 90.01(4) 90.03(6) 89.94(9) V = 1127(2) unit cell: 10.4077(14) 10.4077(14) 10.4077(14) 90.0 90.0 90.0 V = 1127.4(3) Run 8 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.037) HKL list info: 440 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: 0.066076 0.015476 0.005970 ( 0.000100 0.000063 0.000035 ) -0.016423 0.064858 0.013326 ( 0.000084 0.000053 0.000030 ) -0.002601 -0.014364 0.066526 ( 0.000054 0.000034 0.000019 ) M - matrix: 0.004642 -0.000005 0.000003 ( 0.000013 0.000007 0.000004 ) -0.000005 0.004652 0.000001 ( 0.000007 0.000007 0.000003 ) 0.000003 0.000001 0.004639 ( 0.000004 0.000003 0.000003 ) Constraint UB - matrix: 0.066076 0.015476 0.005970 ( 0.000100 0.000063 0.000035 ) -0.016423 0.064858 0.013326 ( 0.000084 0.000053 0.000030 ) -0.002601 -0.014364 0.066526 ( 0.000054 0.000034 0.000019 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 41 obs out of 41 (total:41,skipped:0) (100.00%) unit cell: 10.410(15) 10.399(8) 10.414(3) 90.01(4) 90.03(6) 89.94(9) V = 1127(2) unit cell: 10.4077(14) 10.4077(14) 10.4077(14) 90.0 90.0 90.0 V = 1127.4(3) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_1.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068155 0.000003 -0.000025 ( 0.000009 0.000008 0.000008 ) 0.000000 0.068087 -0.000008 ( 0.000009 0.000009 0.000009 ) 0.000031 -0.000022 0.068163 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000001 0.000001 ) 0.000000 0.004636 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000002 0.004646 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068155 0.000003 -0.000025 ( 0.000009 0.000008 0.000008 ) 0.000000 0.068087 -0.000008 ( 0.000009 0.000009 0.000009 ) 0.000031 -0.000022 0.068163 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) UB fit with 1511 obs out of 1536 (total:1536,skipped:0) (98.37%) unit cell: 10.4072(13) 10.4176(13) 10.4059(10) 89.975(9) 90.005(9) 90.003(10) V = 1128.2(2) unit cell: 10.4102(3) 10.4102(3) 10.4102(3) 90.0 90.0 90.0 V = 1128.19(6) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 191 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_7.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_8.rrpprof 6815 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 15:05:43 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.003) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.037) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.037) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.037) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.040) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) Run 8 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.037) PROFFIT INFO: signal sum: min=-784.0000 max=7912518.0000 PROFFIT INFO: signal sum lp corr: min=-742.7477 max=1263976.4923 PROFFIT INFO: background sum: min=-93.0000 max=8401.0000 PROFFIT INFO: background sum sig2: min=440.0000 max=5744.0000 PROFFIT INFO: num of signal pixels: min=41 max=517 PROFFIT INFO: Inet: min=-1188.3964 max=2022362.3750 PROFFIT INFO: sig(Inet): min=52.0628 max=30728.5625 PROFFIT INFO: Inet/sig(Inet): min=-2.12 max=277.43 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 598 2329 3539 4226 4562 5301 5755 6032 6458 6744 6815 Percent 8.8 34.2 51.9 62.0 66.9 77.8 84.4 88.5 94.8 99.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 6815 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 6815 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2022362- 131259 681 413678.65 77.55 100.00 131175- 4011 681 29015.12 19.34 100.00 3997- 2107 681 2885.57 7.00 97.36 2099- 1242 681 1600.59 3.93 52.13 1241- 819 681 1012.62 2.34 16.30 819- 548 681 678.31 1.73 8.08 548- 341 681 441.00 1.24 5.43 341- 156 681 247.71 0.73 0.88 156- 19 681 82.40 0.29 0.00 19- -1188 686 -142.09 -0.28 0.00 ------------------------------------------------------------------------------------ 2022362- -1188 6815 44916.90 11.38 37.99 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 681 110016.08 15.57 68.43 1.64- 1.26 681 87149.70 21.06 57.86 1.26- 1.06 681 70195.87 20.62 69.46 1.06- 0.96 681 45170.10 12.65 31.57 0.96- 0.88 681 23942.53 8.80 46.70 0.88- 0.80 681 44353.38 12.56 34.21 0.80- 0.75 681 19294.24 5.97 19.82 0.75- 0.71 681 20804.25 6.77 16.45 0.71- 0.67 681 24949.42 8.09 29.22 0.67- 0.63 686 3596.85 1.78 6.41 ------------------------------------------------------------------------------------ 6.00- 0.63 6815 44916.90 11.38 37.99 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 15:05:44 2019 Sorting 6815 observations 53 unique observations with > 7.00 F2/sig(F2) 6815 observations in 8 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 8 0 24 686 Total number of frames 686 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 13 frame = 1 scale 6815 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 3 52 8 0 1 54 Total number of frames 54 1639 observations > 7.00 F2/sig(F2) 1639 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 3 52 8 0 1 54 Total number of frames 54 Removing 'redundancy=1' reflections Average redundancy: 23.6 (Out of 1639 removed 8 = 1631, unique = 69) 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 1631 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 3 52 8 0 1 54 Total number of frames 54 69 unique data precomputed (should be 69) 69 unique data with 1631 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.6 (Out of 1631 removed 0 = 1631, unique = 69) 69 unique data precomputed (should be 69) 69 unique data with 1631 observations RMS deviation of equivalent data = 0.30989 Rint = 0.25337 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24604, wR= 0.33796 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13583, wR= 0.18564, Acormin=0.469, Acormax=1.434, Acor_av=0.999 F test: Probability=1.000, F= 3.271 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13325, wR= 0.17946, Acormin=0.477, Acormax=1.481, Acor_av=0.985 F test: Probability=0.763, F= 1.037 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12838, wR= 0.17599, Acormin=0.551, Acormax=1.549, Acor_av=1.005 F test: Probability=0.982, F= 1.113 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12354, wR= 0.16792, Acormin=0.493, Acormax=1.572, Acor_av=0.993 F test: Probability=0.929, F= 1.078 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10437, wR= 0.14875, Acormin=0.560, Acormax=1.828, Acor_av=1.043 F test: Probability=1.000, F= 1.503 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12197, wR= 0.16872, Acormin=0.428, Acormax=1.633, Acor_av=0.986 F test: Probability=0.000, F= 0.731 Trying model 7 (ne=6, no=1)... Results: Rint= 0.11787, wR= 0.16224, Acormin=0.457, Acormax=1.623, Acor_av=0.982 F test: Probability=0.000, F= 0.781 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09956, wR= 0.14516, Acormin=0.535, Acormax=1.839, Acor_av=1.029 F test: Probability=0.953, F= 1.090 Trying model 9 (ne=6, no=5)... Results: Rint= 0.14579, wR= 0.18973, Acormin=0.131, Acormax=1.112, Acor_av=0.544 F test: Probability=0.000, F= 0.463 Final absorption model (ne=6, no=3): Rint= 0.09956, Acormin=0.535, Acormax=1.839, Acor_av=1.029 Combined refinement in use Rint: 0.25523 There are 54 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 90 pars with 4095 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30989 Using Levenberg-Marquardt: 0.00010 New wR= 0.10806 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25337 with corrections 0.07995 Rint for all data: 0.25523 with corrections 0.08269 4 observations identified as outliers and rejected Cycle 2 wR= 0.09538 Using Levenberg-Marquardt: 0.00001 New wR= 0.07671 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25319 with corrections 0.05339 Rint for all data: 0.25523 with corrections 0.05956 0 observations identified as outliers and rejected Cycle 3 wR= 0.07671 Using Levenberg-Marquardt: 0.00000 New wR= 0.07392 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25319 with corrections 0.05329 Rint for all data: 0.25523 with corrections 0.05933 0 observations identified as outliers and rejected Cycle 4 wR= 0.07392 Using Levenberg-Marquardt: 0.00000 New wR= 0.07303 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25319 with corrections 0.05269 Rint for all data: 0.25523 with corrections 0.05869 0 observations identified as outliers and rejected Cycle 5 wR= 0.07303 Using Levenberg-Marquardt: 0.00000 New wR= 0.07240 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25319 with corrections 0.05241 Rint for all data: 0.25523 with corrections 0.05835 0 observations identified as outliers and rejected Final wR= 0.07240 Final frame scales: Min= 0.6328 Max= 1.1979 Final absorption correction factors: Amin= 0.3233 Amax= 1.6181 PROFFIT INFO: Inet (after scale3 abspack): min=-1131.8499 max=1273648.8750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.0513 max=22746.1563 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/104 6815 reflections read from tmp file 244 reflections are rejected (243 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 4 2 4 4 5 3 3 214 Initial Chi^2= 0.53089 Cycle 1, Chi^2= 1.00750 Current error model SIG(F2)^2 = 58.85*I_RAW + 13.54*I_BACK+(0.03208*)^2 Cycle 2, Chi^2= 1.00951 Current error model SIG(F2)^2 = 71.28*I_RAW + 10.31*I_BACK+(0.02592*)^2 Cycle 3, Chi^2= 1.00452 Current error model SIG(F2)^2 = 76.17*I_RAW + 9.24*I_BACK+(0.02420*)^2 Cycle 4, Chi^2= 1.00158 Current error model SIG(F2)^2 = 77.83*I_RAW + 8.91*I_BACK+(0.02376*)^2 Cycle 5, Chi^2= 1.00048 Current error model SIG(F2)^2 = 78.34*I_RAW + 8.81*I_BACK+(0.02364*)^2 Cycle 6, Chi^2= 1.00014 Current error model SIG(F2)^2 = 78.48*I_RAW + 8.78*I_BACK+(0.02361*)^2 Final Chi^2= 1.00014 Final error model SIG(F2)^2 = 78.48*I_RAW + 8.78*I_BACK+(0.02361*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1273649- 116675 681 377019.19 33.40 100.00 116353- 3451 681 29042.92 13.68 100.00 3427- 2003 681 2671.08 6.41 99.27 2002- 1153 681 1502.98 4.05 69.31 1153- 770 681 948.94 2.84 29.22 770- 518 681 643.48 2.44 16.89 516- 326 681 417.17 1.97 8.96 326- 153 681 241.92 1.44 3.67 153- 20 681 80.79 0.69 0.15 19- -1132 686 -141.63 -0.56 0.00 ------------------------------------------------------------------------------------ 1273649- -1132 6815 41212.32 6.63 42.71 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 681 102511.58 10.83 72.10 1.64- 1.26 681 79825.37 9.96 61.53 1.26- 1.06 681 63820.47 9.60 74.45 1.06- 0.96 681 41684.82 6.27 34.51 0.96- 0.88 681 21812.66 5.86 55.51 0.88- 0.80 681 40518.15 7.23 42.14 0.80- 0.75 681 17766.18 4.15 23.05 0.75- 0.71 681 18536.74 4.99 21.73 0.71- 0.67 681 22535.97 5.73 33.48 0.67- 0.63 686 3388.98 1.74 8.89 ------------------------------------------------------------------------------------ 6.00- 0.63 6815 41212.32 6.63 42.71 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 681 102511.58 10.83 72.10 6.00- 1.26 1362 91168.47 10.39 66.81 6.00- 1.06 2043 82052.47 10.13 69.36 6.00- 0.96 2724 71960.56 9.16 60.65 6.00- 0.88 3405 61930.98 8.50 59.62 6.00- 0.80 4086 58362.17 8.29 56.71 6.00- 0.75 4767 52562.75 7.70 51.90 6.00- 0.71 5448 48309.50 7.36 48.13 6.00- 0.67 6129 45445.77 7.18 46.50 6.00- 0.63 6815 41212.32 6.63 42.71 ------------------------------------------------------------------------------------ 6.00- 0.63 6815 41212.32 6.63 42.71 Scale applied to data: s=0.785145 (maximum obs:1273648.875,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.058; Rsigma 0.035: data 6815 -> merged 240 With outlier rejection... Rint 0.050; Rsigma 0.035: data 6792 -> merged 240 Rejected total: 23, method kkm 10, method Blessing 13 Completeness direct cell (a, b, c) = (10.410, 10.410, 10.410), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626623, 6.010357 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.41 - 1.59 21 21 36.57 100.00 768 1.57 - 1.20 21 21 38.43 100.00 807 1.19 - 1.02 21 21 36.14 100.00 759 1.02 - 0.91 21 21 34.86 100.00 732 0.91 - 0.84 21 21 30.90 100.00 649 0.84 - 0.78 21 21 30.43 100.00 639 0.78 - 0.74 21 21 28.71 100.00 603 0.74 - 0.71 21 21 24.19 100.00 508 0.71 - 0.68 21 21 26.90 100.00 565 0.68 - 0.65 23 23 22.78 100.00 524 --------------------------------------------------------------- 10.41 - 0.65 212 212 30.92 100.00 6554 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 15:05:44 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.407219 10.417619 10.405900 89.9753 90.0051 90.0031 6792 Reflections read from file xs2212a.hkl 6751 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.60 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3385 0 4479 4471 6751 N (int>3sigma) = 0 0 0 0 1546 0 2023 1996 2890 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.0 31.2 31.8 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.7 6.6 6.6 Lattice type: F chosen Volume: 1128.19 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 0.5000 Unitcell: 7.358 7.359 7.361 119.97 119.97 90.01 Niggli form: a.a = 54.143 b.b = 54.153 c.c = 54.179 b.c = -27.060 a.c = -27.058 a.b = -0.007 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.084 CUBIC F-lattice R(int) = 0.050 [ 6520] Vol = 1128.2 Cell: 10.418 10.407 10.406 89.99 90.02 90.00 Volume: 1128.19 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.039 TETRAGONAL I-lattice R(int) = 0.050 [ 6134] Vol = 564.1 Cell: 7.363 7.362 10.406 89.99 89.98 89.94 Volume: 564.10 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.022 TETRAGONAL I-lattice R(int) = 0.049 [ 6134] Vol = 564.1 Cell: 7.358 7.359 10.418 89.98 89.98 90.01 Volume: 564.10 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.088 TETRAGONAL I-lattice R(int) = 0.050 [ 6134] Vol = 564.1 Cell: 7.362 7.363 10.406 90.02 89.99 90.06 Volume: 564.10 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.024 ORTHORHOMBIC F-lattice R(int) = 0.049 [ 6081] Vol = 1128.2 Cell: 10.406 10.407 10.418 90.00 90.02 89.99 Volume: 1128.19 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.055 ORTHORHOMBIC I-lattice R(int) = 0.049 [ 6062] Vol = 564.1 Cell: 10.406 7.362 7.363 89.94 89.98 89.99 Volume: 564.10 Matrix: 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.023 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 6061] Vol = 564.1 Cell: 7.358 7.359 10.418 90.02 90.02 90.01 Volume: 564.10 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.023 MONOCLINIC I-lattice R(int) = 0.047 [ 5535] Vol = 564.1 Cell: 7.362 10.406 7.363 90.02 90.06 89.99 Volume: 564.10 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.010 MONOCLINIC I-lattice R(int) = 0.048 [ 5533] Vol = 564.1 Cell: 7.361 10.407 7.364 89.99 90.06 90.00 Volume: 564.10 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.023 MONOCLINIC I-lattice R(int) = 0.047 [ 5535] Vol = 564.1 Cell: 7.362 10.406 7.363 90.02 90.06 89.99 Volume: 564.10 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.015 MONOCLINIC I-lattice R(int) = 0.047 [ 5518] Vol = 564.1 Cell: 7.359 7.358 10.418 89.98 90.02 89.99 Volume: 564.10 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.018 MONOCLINIC I-lattice R(int) = 0.047 [ 5513] Vol = 564.1 Cell: 7.358 7.359 10.418 89.98 90.02 89.99 Volume: 564.10 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.017 MONOCLINIC I-lattice R(int) = 0.046 [ 5533] Vol = 564.1 Cell: 7.358 10.418 7.359 89.98 90.01 89.98 Volume: 564.10 Matrix: 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.049 MONOCLINIC I-lattice R(int) = 0.046 [ 5533] Vol = 564.1 Cell: 7.358 10.418 7.359 90.02 90.01 90.02 Volume: 564.10 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) = 0.043 [ 4467] Vol = 282.0 Cell: 7.358 7.359 7.361 119.97 119.97 90.01 Volume: 282.05 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 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 3385 0 4479 4471 6751 N (int>3sigma) = 0 0 0 0 1546 0 2023 1996 2890 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.0 31.2 31.8 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.7 6.6 6.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.438 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 49 49 500 1331 N I>3s 2 2 2 720 0.0 0.0 0.0 1.9 0.8 0.8 0.2 5.2 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 0.050 6048 Fd-3m 1 1 227 C N N N N 37 2284 0.050 6110 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.417619 10.407219 10.405900 89.9949 90.0247 90.0031 ZERR 5.00 0.001321 0.001299 0.000990 0.0090 0.0091 0.0102 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1119026- 124491 675 660 26 25.4 376990.26 33.39 0.046 0.060 107918- 3147 767 764 26 29.4 27016.53 12.88 0.060 0.066 3002- 1408 985 982 26 37.8 2220.36 5.80 0.129 0.183 1351- 850 856 856 26 32.9 1049.10 2.85 0.232 0.304 845- 516 830 830 26 31.9 648.25 2.36 0.311 0.422 515- 301 869 869 26 33.4 387.33 1.78 0.431 0.594 291- 137 626 626 26 24.1 218.73 1.26 0.599 1.064 133- 20 643 642 26 24.7 66.57 0.48 0.901 2.666 17- -184 564 563 32 17.6 -29.90 -0.07 0.994 4.358 ------------------------------------------------------------------------------------------- 1119026- -184 6815 6792 240 28.3 40278.28 6.56 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-1.44 989 984 26 37.8 113961.99 12.00 0.049 0.063 0.026 1.39-1.09 1040 1037 26 39.9 43448.54 7.76 0.044 0.061 0.032 1.06-0.94 873 869 26 33.4 37801.13 5.96 0.041 0.051 0.034 0.92-0.84 826 823 26 31.7 40794.71 7.90 0.049 0.061 0.039 0.84-0.78 807 806 26 31.0 24640.57 5.31 0.059 0.079 0.045 0.78-0.73 682 680 26 26.2 7694.24 3.00 0.070 0.082 0.078 0.73-0.69 728 727 27 26.9 19065.30 4.99 0.064 0.075 0.058 0.68-0.66 601 600 26 23.1 15051.10 4.12 0.071 0.093 0.065 0.66-0.63 269 266 31 8.6 7400.79 2.33 0.074 0.064 0.087 ------------------------------------------------------------------------------------------------------ inf-0.63 6815 6792 240 28.3 40278.28 6.56 0.050 0.065 0.035 inf-0.65 6572 6552 211 31.1 41527.41 6.73 0.050 0.064 0.035 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-1.44 984 26 26 100.0 37.8 113961.99 74.18 0.049 0.005 1.39-1.09 1037 26 26 100.0 39.9 43448.54 44.22 0.044 0.006 1.06-0.94 869 26 26 100.0 33.4 37801.13 35.18 0.041 0.007 0.92-0.84 823 26 26 100.0 31.7 40794.71 44.21 0.049 0.008 0.84-0.78 806 26 26 100.0 31.0 24640.57 28.27 0.059 0.008 0.78-0.73 680 26 26 100.0 26.2 7694.24 15.05 0.070 0.015 0.73-0.69 727 27 27 100.0 26.9 19065.30 24.95 0.064 0.012 0.68-0.66 600 26 26 100.0 23.1 15051.10 21.44 0.071 0.014 0.66-0.63 266 31 31 100.0 8.6 7400.79 6.53 0.074 0.033 -------------------------------------------------------------------------------------------- inf-0.63 6792 240 240 100.0 28.3 40278.28 37.04 0.050 0.008 inf-0.65 6552 211 211 100.0 31.1 41527.41 38.18 0.050 0.007 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066102 0.015147 0.006765 ( 0.000008 0.000008 0.000008 ) -0.016228 0.064774 0.013278 ( 0.000009 0.000009 0.000009 ) -0.003476 -0.014497 0.066514 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000001 0.000001 ) 0.000000 0.004635 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000002 0.004646 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066102 0.015147 0.006765 ( 0.000008 0.000008 0.000008 ) -0.016228 0.064774 0.013278 ( 0.000009 0.000009 0.000009 ) -0.003476 -0.014497 0.066514 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4074(13) 10.4183(13) 10.4059(10) 89.979(9) 90.006(9) 90.006(10) V = 1128.3(2) unit cell: 10.4105(3) 10.4105(3) 10.4105(3) 90.0 90.0 90.0 V = 1128.28(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.003) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.037) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.037) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.037) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.040) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) Run 8 Omega scan: (-49.000 - -24.000,25 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.037) PROFFIT INFO: signal sum: min=-784.0000 max=7912518.0000 PROFFIT INFO: signal sum lp corr: min=-742.7477 max=1263976.4923 PROFFIT INFO: background sum: min=-93.0000 max=8401.0000 PROFFIT INFO: background sum sig2: min=440.0000 max=5744.0000 PROFFIT INFO: num of signal pixels: min=41 max=517 PROFFIT INFO: Inet: min=-1188.3964 max=2022362.3750 PROFFIT INFO: sig(Inet): min=52.0628 max=30728.5625 PROFFIT INFO: Inet/sig(Inet): min=-2.12 max=277.43 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 1196 4658 7078 8452 9124 10602 11510 12064 12916 13488 13630 Percent 8.8 34.2 51.9 62.0 66.9 77.8 84.4 88.5 94.8 99.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 6815 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 6815 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2022362- 131259 681 413678.65 77.55 100.00 131175- 4011 681 29015.12 19.34 100.00 3997- 2107 681 2885.57 7.00 97.36 2099- 1242 681 1600.59 3.93 52.13 1241- 819 681 1012.62 2.34 16.30 819- 548 681 678.31 1.73 8.08 548- 341 681 441.00 1.24 5.43 341- 156 681 247.71 0.73 0.88 156- 19 681 82.40 0.29 0.00 19- -1188 686 -142.09 -0.28 0.00 ------------------------------------------------------------------------------------ 2022362- -1188 6815 44916.90 11.38 37.99 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 681 110016.08 15.57 68.43 1.64- 1.26 681 87149.70 21.06 57.86 1.26- 1.06 681 70195.87 20.62 69.46 1.06- 0.96 681 45170.10 12.65 31.57 0.96- 0.88 681 23942.53 8.80 46.70 0.88- 0.80 681 44353.38 12.56 34.21 0.80- 0.75 681 19294.24 5.97 19.82 0.75- 0.71 681 20804.25 6.77 16.45 0.71- 0.67 681 24949.42 8.09 29.22 0.67- 0.63 686 3596.85 1.78 6.41 ------------------------------------------------------------------------------------ 6.00- 0.63 6815 44916.90 11.38 37.99 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 15:05:45 2019 Sorting 6815 observations 43 unique observations with > 7.00 F2/sig(F2) 6815 observations in 8 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 8 0 24 686 Total number of frames 686 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 16 frame = 1 scale 6815 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 2 45 8 0 1 47 Total number of frames 47 1639 observations > 7.00 F2/sig(F2) 1639 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 2 45 8 0 1 47 Total number of frames 47 Removing 'redundancy=1' reflections Average redundancy: 29.2 (Out of 1639 removed 4 = 1635, unique = 56) 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 1635 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 2 45 8 0 1 47 Total number of frames 47 56 unique data precomputed (should be 56) 56 unique data with 1635 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 29.2 (Out of 1635 removed 0 = 1635, unique = 56) 56 unique data precomputed (should be 56) 56 unique data with 1635 observations RMS deviation of equivalent data = 0.31014 Rint = 0.25358 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24625, wR= 0.33819 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13578, wR= 0.18626, Acormin=0.469, Acormax=1.434, Acor_av=0.999 F test: Probability=1.000, F= 3.279 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13315, wR= 0.18007, Acormin=0.478, Acormax=1.481, Acor_av=0.985 F test: Probability=0.769, F= 1.038 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12795, wR= 0.17692, Acormin=0.552, Acormax=1.549, Acor_av=1.006 F test: Probability=0.987, F= 1.120 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12350, wR= 0.16866, Acormin=0.496, Acormax=1.573, Acor_av=0.994 F test: Probability=0.913, F= 1.071 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10435, wR= 0.14939, Acormin=0.562, Acormax=1.829, Acor_av=1.042 F test: Probability=1.000, F= 1.494 Final absorption model (ne=4, no=3): Rint= 0.10435, Acormin=0.562, Acormax=1.829, Acor_av=1.042 Combined refinement in use Rint: 0.25544 There are 47 active scales (one needs to be fixed) Refinement control: frame scale #32 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 70 pars with 2485 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31014 Using Levenberg-Marquardt: 0.00010 New wR= 0.12070 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25358 with corrections 0.08920 Rint for all data: 0.25544 with corrections 0.09186 4 observations identified as outliers and rejected Cycle 2 wR= 0.10864 Using Levenberg-Marquardt: 0.00001 New wR= 0.08927 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25340 with corrections 0.05833 Rint for all data: 0.25544 with corrections 0.06388 0 observations identified as outliers and rejected Cycle 3 wR= 0.08927 Using Levenberg-Marquardt: 0.00000 New wR= 0.08498 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25340 with corrections 0.05588 Rint for all data: 0.25544 with corrections 0.06124 0 observations identified as outliers and rejected Cycle 4 wR= 0.08498 Using Levenberg-Marquardt: 0.00000 New wR= 0.08352 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25340 with corrections 0.05484 Rint for all data: 0.25544 with corrections 0.06000 0 observations identified as outliers and rejected Cycle 5 wR= 0.08352 Using Levenberg-Marquardt: 0.00000 New wR= 0.08255 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25340 with corrections 0.05442 Rint for all data: 0.25544 with corrections 0.05957 0 observations identified as outliers and rejected Final wR= 0.08255 Final frame scales: Min= 0.6607 Max= 1.1642 Final absorption correction factors: Amin= 0.3424 Amax= 1.4907 PROFFIT INFO: Inet (after scale3 abspack): min=-1150.2166 max=1267258.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.0200 max=24065.9297 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/104 6815 reflections read from tmp file 280 reflections are rejected (280 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 3 1 1 4 1 1 0 151 Initial Chi^2= 0.53040 Cycle 1, Chi^2= 1.00033 Current error model SIG(F2)^2 = 61.32*I_RAW + 12.62*I_BACK+(0.03674*)^2 Cycle 2, Chi^2= 1.01023 Current error model SIG(F2)^2 = 76.17*I_RAW + 8.97*I_BACK+(0.02830*)^2 Cycle 3, Chi^2= 1.00610 Current error model SIG(F2)^2 = 82.52*I_RAW + 7.62*I_BACK+(0.02604*)^2 Cycle 4, Chi^2= 1.00221 Current error model SIG(F2)^2 = 84.71*I_RAW + 7.20*I_BACK+(0.02551*)^2 Cycle 5, Chi^2= 1.00067 Current error model SIG(F2)^2 = 85.38*I_RAW + 7.08*I_BACK+(0.02539*)^2 Cycle 6, Chi^2= 1.00019 Current error model SIG(F2)^2 = 85.57*I_RAW + 7.04*I_BACK+(0.02536*)^2 Final Chi^2= 1.00019 Final error model SIG(F2)^2 = 85.57*I_RAW + 7.04*I_BACK+(0.02536*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1267258- 116996 681 377681.41 31.38 100.00 116867- 3428 681 29123.54 13.04 100.00 3426- 2009 681 2668.99 6.16 99.27 2007- 1152 681 1509.03 3.92 64.90 1150- 776 681 951.77 2.77 27.02 776- 517 681 644.33 2.39 15.57 517- 330 681 417.69 1.94 8.52 330- 154 681 242.75 1.45 3.38 153- 20 681 80.80 0.71 0.29 19- -1150 686 -141.80 -0.56 0.00 ------------------------------------------------------------------------------------ 1267258- -1150 6815 41287.43 6.31 41.86 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 681 102597.91 10.25 71.66 1.64- 1.26 681 79240.57 9.44 61.23 1.26- 1.06 681 64060.65 9.10 73.57 1.06- 0.96 681 41600.44 5.95 33.92 0.96- 0.88 681 22192.72 5.60 54.04 0.88- 0.80 681 40857.43 6.88 41.12 0.80- 0.75 681 17795.96 3.98 22.47 0.75- 0.71 681 18761.07 4.79 20.12 0.71- 0.67 681 22635.18 5.49 32.75 0.67- 0.63 686 3410.53 1.69 8.02 ------------------------------------------------------------------------------------ 6.00- 0.63 6815 41287.43 6.31 41.86 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 681 102597.91 10.25 71.66 6.00- 1.26 1362 90919.24 9.85 66.45 6.00- 1.06 2043 81966.37 9.60 68.82 6.00- 0.96 2724 71874.89 8.69 60.10 6.00- 0.88 3405 61938.46 8.07 58.88 6.00- 0.80 4086 58424.95 7.87 55.92 6.00- 0.75 4767 52620.81 7.32 51.14 6.00- 0.71 5448 48388.34 7.00 47.27 6.00- 0.67 6129 45526.88 6.83 45.65 6.00- 0.63 6815 41287.43 6.31 41.86 ------------------------------------------------------------------------------------ 6.00- 0.63 6815 41287.43 6.31 41.86 Scale applied to data: s=0.789104 (maximum obs:1267258.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.060; Rsigma 0.037: data 6815 -> merged 162 With outlier rejection... Rint 0.054; Rsigma 0.037: data 6800 -> merged 162 Rejected total: 15, method kkm 5, method Blessing 10 Completeness direct cell (a, b, c) = (10.411, 10.411, 10.411), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626639, 6.010513 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.41 - 1.76 14 14 44.00 100.00 616 1.74 - 1.27 14 14 48.14 100.00 674 1.26 - 1.06 14 14 55.00 100.00 770 1.05 - 0.97 14 14 47.93 100.00 671 0.95 - 0.88 14 14 50.21 100.00 703 0.87 - 0.81 14 14 44.86 100.00 628 0.80 - 0.76 14 14 47.07 100.00 659 0.76 - 0.72 14 14 38.71 100.00 542 0.72 - 0.69 14 14 43.57 100.00 610 0.69 - 0.65 19 19 36.16 100.00 687 --------------------------------------------------------------- 10.41 - 0.65 145 145 45.24 100.00 6560 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 15:05:44 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.407219 10.417619 10.405900 89.9753 90.0051 90.0031 6792 Reflections read from file xs2212a.hkl 6751 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.60 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3385 0 4479 4471 6751 N (int>3sigma) = 0 0 0 0 1546 0 2023 1996 2890 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.0 31.2 31.8 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.7 6.6 6.6 Lattice type: F chosen Volume: 1128.19 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 0.5000 Unitcell: 7.358 7.359 7.361 119.97 119.97 90.01 Niggli form: a.a = 54.143 b.b = 54.153 c.c = 54.179 b.c = -27.060 a.c = -27.058 a.b = -0.007 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.084 CUBIC F-lattice R(int) = 0.050 [ 6520] Vol = 1128.2 Cell: 10.418 10.407 10.406 89.99 90.02 90.00 Volume: 1128.19 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.039 TETRAGONAL I-lattice R(int) = 0.050 [ 6134] Vol = 564.1 Cell: 7.363 7.362 10.406 89.99 89.98 89.94 Volume: 564.10 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.022 TETRAGONAL I-lattice R(int) = 0.049 [ 6134] Vol = 564.1 Cell: 7.358 7.359 10.418 89.98 89.98 90.01 Volume: 564.10 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.088 TETRAGONAL I-lattice R(int) = 0.050 [ 6134] Vol = 564.1 Cell: 7.362 7.363 10.406 90.02 89.99 90.06 Volume: 564.10 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.024 ORTHORHOMBIC F-lattice R(int) = 0.049 [ 6081] Vol = 1128.2 Cell: 10.406 10.407 10.418 90.00 90.02 89.99 Volume: 1128.19 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.055 ORTHORHOMBIC I-lattice R(int) = 0.049 [ 6062] Vol = 564.1 Cell: 10.406 7.362 7.363 89.94 89.98 89.99 Volume: 564.10 Matrix: 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.023 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 6061] Vol = 564.1 Cell: 7.358 7.359 10.418 90.02 90.02 90.01 Volume: 564.10 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.023 MONOCLINIC I-lattice R(int) = 0.047 [ 5535] Vol = 564.1 Cell: 7.362 10.406 7.363 90.02 90.06 89.99 Volume: 564.10 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.010 MONOCLINIC I-lattice R(int) = 0.048 [ 5533] Vol = 564.1 Cell: 7.361 10.407 7.364 89.99 90.06 90.00 Volume: 564.10 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.023 MONOCLINIC I-lattice R(int) = 0.047 [ 5535] Vol = 564.1 Cell: 7.362 10.406 7.363 90.02 90.06 89.99 Volume: 564.10 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.015 MONOCLINIC I-lattice R(int) = 0.047 [ 5518] Vol = 564.1 Cell: 7.359 7.358 10.418 89.98 90.02 89.99 Volume: 564.10 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.018 MONOCLINIC I-lattice R(int) = 0.047 [ 5513] Vol = 564.1 Cell: 7.358 7.359 10.418 89.98 90.02 89.99 Volume: 564.10 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.017 MONOCLINIC I-lattice R(int) = 0.046 [ 5533] Vol = 564.1 Cell: 7.358 10.418 7.359 89.98 90.01 89.98 Volume: 564.10 Matrix: 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.049 MONOCLINIC I-lattice R(int) = 0.046 [ 5533] Vol = 564.1 Cell: 7.358 10.418 7.359 90.02 90.01 90.02 Volume: 564.10 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) = 0.043 [ 4467] Vol = 282.0 Cell: 7.358 7.359 7.361 119.97 119.97 90.01 Volume: 282.05 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 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 3385 0 4479 4471 6751 N (int>3sigma) = 0 0 0 0 1546 0 2023 1996 2890 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.0 31.2 31.8 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.7 6.6 6.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.438 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 49 49 500 1331 N I>3s 2 2 2 720 0.0 0.0 0.0 1.9 0.8 0.8 0.2 5.2 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 0.050 6048 Fd-3m 1 1 227 C N N N N 37 2284 0.050 6110 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.417619 10.407219 10.405900 89.9949 90.0247 90.0031 ZERR 5.00 0.001321 0.001299 0.000990 0.0090 0.0091 0.0102 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1127794- 93189 826 817 27 30.3 328188.61 29.46 0.050 0.066 80378- 1768 1282 1278 27 47.3 5208.12 8.26 0.088 0.096 1631- 755 1381 1380 27 51.1 1124.04 2.98 0.227 0.301 748- 329 1348 1348 27 49.9 494.59 1.99 0.370 0.527 324- 75 957 957 27 35.4 209.06 1.15 0.626 1.250 67- -158 1021 1020 27 37.8 9.90 0.18 0.963 3.839 ------------------------------------------------------------------------------------------- 1127794- -158 6815 6800 162 42.0 40766.78 6.28 0.054 0.070 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-1.27 1294 1288 27 47.7 93956.22 10.21 0.049 0.064 0.029 1.26-0.97 1445 1441 28 51.5 49108.34 7.10 0.048 0.060 0.034 0.95-0.81 1333 1331 28 47.5 32189.49 6.36 0.062 0.081 0.043 0.80-0.73 1176 1175 27 43.5 18172.52 4.35 0.063 0.083 0.054 0.72-0.67 1045 1044 27 38.7 18220.90 4.61 0.077 0.101 0.063 0.66-0.63 522 521 25 20.8 4249.23 1.82 0.115 0.092 0.121 ------------------------------------------------------------------------------------------------------ inf-0.63 6815 6800 162 42.0 40766.78 6.28 0.054 0.070 0.037 inf-0.65 6572 6558 144 45.5 42028.29 6.44 0.054 0.069 0.037 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-1.27 1288 27 27 100.0 47.7 93956.22 67.55 0.049 0.006 1.26-0.97 1441 28 28 100.0 51.5 49108.34 47.76 0.048 0.006 0.95-0.81 1331 28 28 100.0 47.5 32189.49 44.14 0.062 0.008 0.80-0.73 1175 27 27 100.0 43.5 18172.52 26.09 0.063 0.010 0.72-0.67 1044 27 27 100.0 38.7 18220.90 30.42 0.077 0.011 0.66-0.63 521 25 25 100.0 20.8 4249.23 8.30 0.115 0.029 -------------------------------------------------------------------------------------------- inf-0.63 6800 162 162 100.0 42.0 40766.78 41.37 0.054 0.007 inf-0.65 6558 144 144 100.0 45.5 42028.29 42.65 0.054 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 15:12:06 2019) ID: 3668; threads 40; handles 811; mem 514544.00 (1204692.00)kB; time: 1w 5d 1h 22m 54s MEMORY INFO: Memory PF:225.0, Ph:555.0, V:1176.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:502.5,peak PF: 700.2, WS: 470.9, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:227.0, Ph:557.0, V:1178.0; MEMORY INFO: Process info - Handles: 812, Memory: PF:504.3,peak PF: 700.2, WS: 472.7, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 15:12:06 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000012 0.000013 0.000012 ) -0.015931 0.064696 0.013068 ( 0.000011 0.000012 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000015 ) 10.42433 ( 0.00182 ) 10.43788 ( 0.00184 ) 10.40727 ( 0.00224 ) 89.88512 ( 0.01598 ) 89.79539 ( 0.01576 ) 90.20497 ( 0.01427 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 15:12:06 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000012 0.000013 0.000012 ) -0.015931 0.064696 0.013068 ( 0.000011 0.000012 0.000012 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004647 -0.000001 -0.000006 ( 0.000002 0.000001 0.000001 ) -0.000001 0.004642 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000006 -0.000003 0.004644 ( 0.000001 0.000001 0.000002 ) unit cell: 10.4243(18) 10.4379(18) 10.407(2) 89.885(16) 89.795(16) 90.205(14) V = 1132.4(4) unit cell: 10.4080(6) 10.4080(6) 10.4080(6) 90.0 90.0 90.0 V = 1127.48(11) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.938 ( 0.170) | 0.923 ( 0.398) | 1.01- 0.88 | 22 | 0.957 ( 0.073) | 1.004 ( 0.124) | 1.180 ( 0.493) | 0.88- 0.79 | 22 | 0.985 ( 0.059) | 1.028 ( 0.140) | 1.234 ( 0.387) | 0.79- 0.70 | 22 | 0.984 ( 0.041) | 0.962 ( 0.107) | 1.276 ( 0.475) | 0.70- 0.63 | 22 | 0.943 ( 0.038) | 0.917 ( 0.081) | 1.311 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 220 | 0.933 ( 0.193) | 0.943 ( 0.158) | 1.113 ( 0.914) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 253 peaks identified as outliers and rejected 253 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 253 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 253 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.86 | 25 | 0.946 ( 0.067) | 0.942 ( 0.097) | 1.046 ( 0.420) | 0.82- 0.73 | 25 | 0.957 ( 0.050) | 0.911 ( 0.086) | 1.356 ( 0.420) | 0.73- 0.63 | 28 | 0.929 ( 0.038) | 0.881 ( 0.096) | 1.353 ( 0.467) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 253 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.060 ( 0.485) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.156) HKL list info: 1283 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 192 peaks identified as outliers and rejected 192 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 192 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 192 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.97 | 19 | 0.842 ( 0.116) | 0.844 ( 0.171) | 0.956 ( 0.449) | 2.63- 1.84 | 19 | 0.822 ( 0.111) | 0.843 ( 0.187) | 0.847 ( 0.504) | 1.84- 1.59 | 19 | 0.842 ( 0.108) | 0.837 ( 0.164) | 0.836 ( 0.354) | 1.59- 1.36 | 19 | 0.936 ( 0.096) | 0.973 ( 0.144) | 0.805 ( 0.268) | 1.36- 1.20 | 19 | 0.950 ( 0.102) | 0.972 ( 0.160) | 0.845 ( 0.330) | 1.20- 1.01 | 19 | 0.995 ( 0.078) | 1.010 ( 0.137) | 1.101 ( 0.434) | 1.01- 0.88 | 19 | 0.998 ( 0.085) | 1.016 ( 0.121) | 1.030 ( 0.364) | 0.88- 0.79 | 19 | 1.037 ( 0.059) | 1.056 ( 0.123) | 0.938 ( 0.316) | 0.79- 0.72 | 19 | 1.031 ( 0.054) | 0.994 ( 0.144) | 1.279 ( 0.526) | 0.70- 0.63 | 21 | 0.975 ( 0.052) | 0.883 ( 0.059) | 1.164 ( 0.415) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 192 | 0.943 ( 0.117) | 0.942 ( 0.164) | 0.982 ( 0.432) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) UB - matrix: 0.065810 0.015591 0.006262 ( 0.000023 0.000019 0.000022 ) -0.016403 0.064531 0.013131 ( 0.000023 0.000020 0.000022 ) -0.002751 -0.014148 0.066421 ( 0.000026 0.000022 0.000025 ) M - matrix: 0.004608 0.000006 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004607 0.000005 ( 0.000002 0.000003 0.000002 ) 0.000014 0.000005 0.004623 ( 0.000002 0.000002 0.000003 ) unit cell: 10.450(3) 10.450(3) 10.432(4) 90.07(3) 90.17(3) 90.08(3) V = 1139.1(6) OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 1279 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 190 peaks identified as outliers and rejected 190 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 190 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 190 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 3.00 | 19 | 0.846 ( 0.114) | 0.847 ( 0.168) | 0.873 ( 0.501) | 2.99- 2.00 | 19 | 0.802 ( 0.108) | 0.800 ( 0.186) | 0.843 ( 0.452) | 1.84- 1.59 | 19 | 0.842 ( 0.097) | 0.828 ( 0.155) | 0.880 ( 0.351) | 1.59- 1.36 | 19 | 0.948 ( 0.083) | 0.983 ( 0.140) | 0.851 ( 0.258) | 1.36- 1.19 | 19 | 0.950 ( 0.094) | 0.960 ( 0.152) | 0.768 ( 0.211) | 1.19- 1.00 | 19 | 1.018 ( 0.060) | 1.041 ( 0.127) | 1.085 ( 0.364) | 1.00- 0.88 | 19 | 1.010 ( 0.085) | 1.031 ( 0.121) | 1.045 ( 0.373) | 0.88- 0.78 | 19 | 1.033 ( 0.056) | 1.044 ( 0.117) | 0.953 ( 0.322) | 0.78- 0.69 | 19 | 1.031 ( 0.055) | 1.004 ( 0.165) | 1.278 ( 0.531) | 0.69- 0.63 | 19 | 0.970 ( 0.050) | 0.876 ( 0.055) | 1.127 ( 0.364) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 190 | 0.945 ( 0.116) | 0.942 ( 0.169) | 0.970 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 UB - matrix: 0.066110 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) UB - matrix: 0.066109 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) 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= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 100 peaks identified as outliers and rejected 100 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 100 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 100 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 2.37 | 10 | 0.824 ( 0.107) | 0.789 ( 0.168) | 0.948 ( 0.526) | 2.13- 1.65 | 10 | 0.887 ( 0.099) | 0.902 ( 0.146) | 0.800 ( 0.370) | 1.64- 1.46 | 10 | 0.917 ( 0.142) | 0.896 ( 0.234) | 0.948 ( 0.416) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.161) | 1.038 ( 0.459) | 1.23- 1.11 | 10 | 1.014 ( 0.089) | 1.022 ( 0.172) | 1.004 ( 0.500) | 1.11- 1.00 | 10 | 0.988 ( 0.107) | 1.011 ( 0.206) | 0.971 ( 0.392) | 1.00- 0.89 | 10 | 1.016 ( 0.106) | 1.093 ( 0.173) | 0.829 ( 0.141) | 0.89- 0.86 | 10 | 0.995 ( 0.094) | 1.038 ( 0.093) | 1.245 ( 0.487) | 0.82- 0.73 | 10 | 1.072 ( 0.046) | 1.130 ( 0.142) | 0.868 ( 0.108) | 0.72- 0.64 | 10 | 1.031 ( 0.064) | 1.069 ( 0.171) | 1.233 ( 0.765) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 0.64 | 100 | 0.972 ( 0.121) | 0.995 ( 0.197) | 0.988 ( 0.476) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) UB - matrix: 0.065966 0.015448 0.005965 ( 0.000053 0.000028 0.000028 ) -0.016426 0.064502 0.013369 ( 0.000054 0.000029 0.000028 ) -0.002418 -0.014553 0.066425 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004627 -0.000005 0.000013 ( 0.000007 0.000004 0.000003 ) -0.000005 0.004611 -0.000012 ( 0.000004 0.000004 0.000002 ) 0.000013 -0.000012 0.004627 ( 0.000003 0.000002 0.000002 ) unit cell: 10.427(8) 10.446(5) 10.428(3) 89.85(3) 90.16(4) 89.93(5) V = 1136(1) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) 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! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 101 peaks identified as outliers and rejected 101 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 101 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 101 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.38 | 10 | 0.825 ( 0.107) | 0.790 ( 0.169) | 1.019 ( 0.527) | 2.13- 1.64 | 10 | 0.860 ( 0.122) | 0.859 ( 0.190) | 0.860 ( 0.389) | 1.64- 1.46 | 10 | 0.944 ( 0.113) | 0.943 ( 0.190) | 0.940 ( 0.402) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.160) | 1.023 ( 0.449) | 1.23- 1.11 | 10 | 1.002 ( 0.107) | 0.995 ( 0.210) | 0.997 ( 0.506) | 1.09- 1.00 | 10 | 1.034 ( 0.082) | 1.115 ( 0.140) | 0.886 ( 0.284) | 0.97- 0.88 | 10 | 0.989 ( 0.091) | 1.159 ( 0.229) | 0.740 ( 0.286) | 0.88- 0.86 | 10 | 1.009 ( 0.084) | 1.059 ( 0.096) | 1.119 ( 0.453) | 0.82- 0.73 | 10 | 1.071 ( 0.046) | 1.128 ( 0.142) | 0.868 ( 0.110) | 0.72- 0.63 | 11 | 1.023 ( 0.066) | 1.042 ( 0.168) | 1.108 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.63 | 101 | 0.974 ( 0.119) | 1.009 ( 0.206) | 0.958 ( 0.416) | 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_8_26.rpb PROFFITPEAK info: 181 peaks in the peak location table UB fit with 78 obs out of 108 (total:108,skipped:0) (72.22%) UB - matrix: 0.065918 0.015269 0.006435 ( 0.000148 0.000085 0.000063 ) -0.016560 0.064730 0.013325 ( 0.000093 0.000053 0.000040 ) -0.003363 -0.014221 0.066532 ( 0.000154 0.000088 0.000066 ) M - matrix: 0.004631 -0.000018 -0.000020 ( 0.000020 0.000009 0.000011 ) -0.000018 0.004625 0.000015 ( 0.000009 0.000008 0.000007 ) -0.000020 0.000015 0.004646 ( 0.000011 0.000007 0.000009 ) unit cell: 10.42(2) 10.430(9) 10.407(10) 90.18(9) 89.75(13) 89.78(11) V = 1131(3) UB fit with 78 obs out of 108 (total:108,skipped:0) (72.22%) UB - matrix: 0.065918 0.015269 0.006435 ( 0.000148 0.000085 0.000063 ) -0.016560 0.064730 0.013325 ( 0.000093 0.000053 0.000040 ) -0.003363 -0.014221 0.066532 ( 0.000154 0.000088 0.000066 ) M - matrix: 0.004631 -0.000018 -0.000020 ( 0.000020 0.000009 0.000011 ) -0.000018 0.004625 0.000015 ( 0.000009 0.000008 0.000007 ) -0.000020 0.000015 0.004646 ( 0.000011 0.000007 0.000009 ) unit cell: 10.42(2) 10.430(9) 10.407(10) 90.18(9) 89.75(13) 89.78(11) V = 1131(3) OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 No constraint UB - matrix: 0.065804 0.015477 0.006022 ( 0.000095 0.000051 0.000045 ) -0.016445 0.064648 0.013333 ( 0.000069 0.000037 0.000033 ) -0.002462 -0.014511 0.066347 ( 0.000067 0.000036 0.000032 ) M - matrix: 0.004607 -0.000009 0.000014 ( 0.000013 0.000006 0.000005 ) -0.000009 0.004629 -0.000008 ( 0.000006 0.000005 0.000003 ) 0.000014 -0.000008 0.004616 ( 0.000005 0.000003 0.000004 ) Constraint UB - matrix: 0.065804 0.015477 0.006022 ( 0.000095 0.000051 0.000045 ) -0.016445 0.064648 0.013333 ( 0.000069 0.000037 0.000033 ) -0.002462 -0.014511 0.066347 ( 0.000067 0.000036 0.000032 ) M - matrix: 0.004618 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004618 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004618 ( 0.000000 0.000000 0.000002 ) UB fit with 104 obs out of 108 (total:108,skipped:0) (96.30%) unit cell: 10.451(14) 10.425(6) 10.440(5) 89.91(4) 90.17(7) 89.89(7) V = 1137(2) unit cell: 10.438(2) 10.438(2) 10.438(2) 90.0 90.0 90.0 V = 1137.4(4) UB fit with 104 obs out of 108 (total:108,skipped:0) (96.30%) UB - matrix: 0.065804 0.015477 0.006022 ( 0.000095 0.000051 0.000045 ) -0.016445 0.064648 0.013333 ( 0.000069 0.000037 0.000033 ) -0.002462 -0.014511 0.066347 ( 0.000067 0.000036 0.000032 ) M - matrix: 0.004607 -0.000009 0.000014 ( 0.000013 0.000006 0.000005 ) -0.000009 0.004629 -0.000008 ( 0.000006 0.000005 0.000003 ) 0.000014 -0.000008 0.004616 ( 0.000005 0.000003 0.000004 ) unit cell: 10.451(14) 10.425(6) 10.440(5) 89.91(4) 90.17(7) 89.89(7) V = 1137(2) OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 OTKP changes: 45 1 1 1 108 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_8" Run 8 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.156) HKL list info: 738 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065804 0.015477 0.006022 ( 0.000095 0.000051 0.000045 ) -0.016445 0.064648 0.013333 ( 0.000069 0.000037 0.000033 ) -0.002462 -0.014511 0.066347 ( 0.000067 0.000036 0.000032 ) M - matrix: 0.004607 -0.000009 0.000014 ( 0.000013 0.000006 0.000005 ) -0.000009 0.004629 -0.000008 ( 0.000006 0.000005 0.000003 ) 0.000014 -0.000008 0.004616 ( 0.000005 0.000003 0.000004 ) Constraint UB - matrix: 0.065804 0.015477 0.006022 ( 0.000095 0.000051 0.000045 ) -0.016445 0.064648 0.013333 ( 0.000069 0.000037 0.000033 ) -0.002462 -0.014511 0.066347 ( 0.000067 0.000036 0.000032 ) M - matrix: 0.004618 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004618 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004618 ( 0.000000 0.000000 0.000002 ) UB fit with 104 obs out of 108 (total:108,skipped:0) (96.30%) unit cell: 10.451(14) 10.425(6) 10.440(5) 89.91(4) 90.17(7) 89.89(7) V = 1137(2) unit cell: 10.438(2) 10.438(2) 10.438(2) 90.0 90.0 90.0 V = 1137.4(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 104 obs out of 108 (total:108,skipped:0) (96.30%) 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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_26.rpb 0 of 103 peaks identified as outliers and rejected 103 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" 103 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8.tabbin file 103 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.93- 2.37 | 10 | 0.838 ( 0.093) | 0.813 ( 0.161) | 0.881 ( 0.450) | 2.14- 1.75 | 10 | 0.845 ( 0.111) | 0.841 ( 0.179) | 0.679 ( 0.189) | 1.65- 1.51 | 10 | 0.945 ( 0.108) | 0.983 ( 0.167) | 0.847 ( 0.457) | 1.50- 1.36 | 10 | 0.988 ( 0.096) | 1.051 ( 0.156) | 0.671 ( 0.252) | 1.23- 1.17 | 10 | 0.994 ( 0.094) | 1.003 ( 0.172) | 0.846 ( 0.379) | 1.15- 1.07 | 10 | 0.963 ( 0.090) | 0.969 ( 0.178) | 0.808 ( 0.314) | 1.07- 0.89 | 10 | 1.030 ( 0.055) | 1.075 ( 0.126) | 1.151 ( 0.424) | 0.89- 0.82 | 10 | 1.037 ( 0.076) | 1.043 ( 0.125) | 1.140 ( 0.369) | 0.82- 0.72 | 10 | 1.047 ( 0.055) | 1.051 ( 0.113) | 0.981 ( 0.152) | 0.72- 0.63 | 13 | 1.007 ( 0.061) | 0.947 ( 0.132) | 1.390 ( 0.577) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.93- 0.63 | 103 | 0.970 ( 0.111) | 0.977 ( 0.174) | 0.953 ( 0.446) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" UB fit with 103 obs out of 103 (total:103,skipped:0) (100.00%) UB - matrix: 0.065827 0.015535 0.005883 ( 0.000059 0.000031 0.000028 ) -0.016543 0.064551 0.013283 ( 0.000057 0.000030 0.000027 ) -0.002491 -0.014435 0.066448 ( 0.000032 0.000017 0.000015 ) M - matrix: 0.004613 -0.000009 0.000002 ( 0.000008 0.000004 0.000003 ) -0.000009 0.004616 -0.000010 ( 0.000004 0.000004 0.000002 ) 0.000002 -0.000010 0.004626 ( 0.000003 0.000002 0.000002 ) unit cell: 10.443(9) 10.439(5) 10.428(2) 89.87(3) 90.03(4) 89.89(5) V = 1137(1) OTKP changes: 103 1 1 1 OTKP changes: 103 1 1 1 OTKP changes: 103 1 1 1 No constraint UB - matrix: 0.065878 0.015540 0.005987 ( 0.000046 0.000024 0.000022 ) -0.016534 0.064733 0.013362 ( 0.000041 0.000022 0.000020 ) -0.002467 -0.014490 0.066429 ( 0.000030 0.000016 0.000014 ) M - matrix: 0.004619 -0.000011 0.000010 ( 0.000006 0.000003 0.000003 ) -0.000011 0.004642 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000010 -0.000005 0.004627 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.065878 0.015540 0.005987 ( 0.000046 0.000024 0.000022 ) -0.016534 0.064733 0.013362 ( 0.000041 0.000022 0.000020 ) -0.002467 -0.014490 0.066429 ( 0.000030 0.000016 0.000014 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000001 ) UB fit with 103 obs out of 103 (total:103,skipped:0) (100.00%) unit cell: 10.436(7) 10.411(4) 10.427(2) 89.94(2) 90.12(3) 89.87(4) V = 1132.9(9) unit cell: 10.4248(10) 10.4248(10) 10.4248(10) 90.0 90.0 90.0 V = 1132.92(19) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.156) HKL list info: 738 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065878 0.015540 0.005987 ( 0.000046 0.000024 0.000022 ) -0.016534 0.064733 0.013362 ( 0.000041 0.000022 0.000020 ) -0.002467 -0.014490 0.066429 ( 0.000030 0.000016 0.000014 ) M - matrix: 0.004619 -0.000011 0.000010 ( 0.000006 0.000003 0.000003 ) -0.000011 0.004642 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000010 -0.000005 0.004627 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.065878 0.015540 0.005987 ( 0.000046 0.000024 0.000022 ) -0.016534 0.064733 0.013362 ( 0.000041 0.000022 0.000020 ) -0.002467 -0.014490 0.066429 ( 0.000030 0.000016 0.000014 ) M - matrix: 0.004631 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004631 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004631 ( 0.000000 0.000000 0.000001 ) UB fit with 103 obs out of 103 (total:103,skipped:0) (100.00%) unit cell: 10.436(7) 10.411(4) 10.427(2) 89.94(2) 90.12(3) 89.87(4) V = 1132.9(9) unit cell: 10.4248(10) 10.4248(10) 10.4248(10) 90.0 90.0 90.0 V = 1132.92(19) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 103 obs out of 103 (total:103,skipped:0) (100.00%) 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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_26.rpb 0 of 102 peaks identified as outliers and rejected 102 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" 102 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8.tabbin file 102 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.02- 2.38 | 10 | 0.846 ( 0.098) | 0.820 ( 0.170) | 0.865 ( 0.535) | 2.38- 1.76 | 10 | 0.837 ( 0.125) | 0.841 ( 0.197) | 0.698 ( 0.179) | 1.76- 1.57 | 10 | 1.091 ( 0.513) | 1.182 ( 0.680) | 1.420 ( 2.106) | 1.50- 1.35 | 10 | 1.000 ( 0.094) | 1.054 ( 0.159) | 0.735 ( 0.236) | 1.35- 1.16 | 10 | 1.005 ( 0.075) | 1.027 ( 0.150) | 0.842 ( 0.378) | 1.15- 1.06 | 10 | 0.955 ( 0.081) | 0.944 ( 0.166) | 0.770 ( 0.292) | 1.06- 0.89 | 10 | 1.039 ( 0.052) | 1.083 ( 0.124) | 1.079 ( 0.400) | 0.89- 0.82 | 10 | 1.042 ( 0.075) | 1.052 ( 0.130) | 1.222 ( 0.369) | 0.82- 0.73 | 10 | 1.046 ( 0.053) | 1.062 ( 0.130) | 0.954 ( 0.188) | 0.72- 0.63 | 12 | 0.997 ( 0.056) | 0.958 ( 0.132) | 1.418 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.02- 0.63 | 102 | 0.986 ( 0.195) | 1.001 ( 0.278) | 1.009 ( 0.794) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.3 | 160 | 1.005 ( 0.134) | 1.058 ( 0.182) | 1.144 ( 0.708) | 10.3-15.2 | 160 | 0.999 ( 0.051) | 1.056 ( 0.073) | 1.083 ( 0.498) | 15.2-19.3 | 160 | 0.998 ( 0.170) | 1.042 ( 0.101) | 1.111 ( 0.909) | 19.4-23.6 | 160 | 0.973 ( 0.067) | 1.013 ( 0.089) | 0.935 ( 0.406) | 23.7-27.6 | 160 | 0.977 ( 0.071) | 1.019 ( 0.118) | 0.966 ( 0.449) | 27.6-32.6 | 160 | 0.951 ( 0.086) | 0.967 ( 0.119) | 0.931 ( 0.430) | 32.7-36.3 | 160 | 0.923 ( 0.151) | 0.913 ( 0.152) | 1.057 ( 0.635) | 36.4-38.9 | 160 | 0.893 ( 0.110) | 0.883 ( 0.240) | 1.006 ( 0.479) | 38.9-42.0 | 160 | 0.898 ( 0.111) | 0.850 ( 0.157) | 0.985 ( 0.441) | 42.0-50.2 | 158 | 0.867 ( 0.125) | 0.790 ( 0.148) | 0.939 ( 0.437) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.2 | 1598 | 0.949 ( 0.123) | 0.959 ( 0.171) | 1.016 ( 0.566) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.14 e2 dimension: a=-0.0068 b=1.24 e3 dimension: a=-0.0000 b=1.11 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_8" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 5011 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 15:12:29 2019 PROFFITMAIN - Started at Wed Aug 21 15:12:29 2019 OTKP changes: 1246 2 7 8 OTKP changes: 1246 2 7 8 OTKP changes: 1246 2 7 8 No constraint UB - matrix: 0.066182 0.015177 0.006649 ( 0.000012 0.000012 0.000012 ) -0.016262 0.064842 0.013209 ( 0.000011 0.000011 0.000011 ) -0.003447 -0.014405 0.066498 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004656 -0.000000 -0.000004 ( 0.000002 0.000001 0.000001 ) -0.000000 0.004642 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000004 -0.000000 0.004641 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066182 0.015177 0.006649 ( 0.000012 0.000012 0.000012 ) -0.016262 0.064842 0.013209 ( 0.000011 0.000011 0.000011 ) -0.003447 -0.014405 0.066498 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000001 ) UB fit with 1314 obs out of 1598 (total:1598,skipped:0) (82.23%) unit cell: 10.3945(18) 10.4103(18) 10.412(2) 89.994(16) 89.951(16) 89.995(14) V = 1126.7(4) unit cell: 10.4056(6) 10.4056(6) 10.4056(6) 90.0 90.0 90.0 V = 1126.70(11) *** 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 187 obs out of 220 (total:220,skipped:0) (85.00%) UB - matrix: 0.066500 0.011702 0.008960 ( 0.000032 0.000043 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000030 0.000040 0.000034 ) -0.006052 -0.013931 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.60(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004603 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 220 (total:220,skipped:0) (85.91%) unit cell: 10.406(5) 10.502(6) 10.456(6) 90.61(5) 90.19(4) 89.64(4) V = 1143(1) unit cell: 10.4543(19) 10.4543(19) 10.4543(19) 90.0 90.0 90.0 V = 1142.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 220 (total:220,skipped:0) (92.27%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004644 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 220 (total:220,skipped:0) (93.64%) unit cell: 10.409(4) 10.492(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1140.0(9) unit cell: 10.4466(13) 10.4466(13) 10.4466(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) UB - matrix: 0.066336 0.014185 0.006781 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064703 0.012861 ( 0.000017 0.000023 0.000023 ) -0.004076 -0.014198 0.066902 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 253 1 1 1 OTKP changes: 253 1 1 1 No constraint UB - matrix: 0.066343 0.014186 0.006784 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014200 0.066900 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066343 0.014186 0.006784 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014200 0.066900 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.11(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066343 0.014186 0.006784 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014200 0.066900 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066343 0.014186 0.006784 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014200 0.066900 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.11(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068244 -0.000102 -0.000276 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000012 0.000000 0.068378 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068244 -0.000102 -0.000276 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000012 0.000000 0.068378 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 253 obs out of 253 (total:253,skipped:0) (100.00%) unit cell: 10.394(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4048(5) 10.4048(5) 10.4048(5) 90.0 90.0 90.0 V = 1126.41(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065883 0.015205 0.006813 ( 0.000019 0.000013 0.000019 ) -0.016066 0.064794 0.013226 ( 0.000017 0.000012 0.000017 ) -0.003636 -0.014499 0.066501 ( 0.000021 0.000015 0.000021 ) M - matrix: 0.004612 0.000013 -0.000005 ( 0.000003 0.000001 0.000002 ) 0.000013 0.004640 -0.000004 ( 0.000001 0.000002 0.000002 ) -0.000005 -0.000004 0.004644 ( 0.000002 0.000002 0.000003 ) unit cell: 10.445(3) 10.413(2) 10.409(3) 89.955(19) 89.93(2) 90.167(19) V = 1132.1(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065936 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064848 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066577 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065936 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064848 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066577 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4059(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.9(5) unit cell: 10.4125(5) 10.4125(5) 10.4125(5) 90.0 90.0 90.0 V = 1128.94(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.032) HKL list info: 1274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065936 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064848 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066577 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065936 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064848 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066577 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4059(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.9(5) unit cell: 10.4125(5) 10.4125(5) 10.4125(5) 90.0 90.0 90.0 V = 1128.94(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065936 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064848 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066577 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004646 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065936 0.015226 0.006784 ( 0.000020 0.000014 0.000019 ) -0.016123 0.064848 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003638 -0.014463 0.066577 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.435(3) 10.4059(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.9(5) unit cell: 10.4125(5) 10.4125(5) 10.4125(5) 90.0 90.0 90.0 V = 1128.94(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066119 0.015253 0.006579 ( 0.000015 0.000020 0.000017 ) -0.016333 0.064737 0.012926 ( 0.000012 0.000015 0.000013 ) -0.003347 -0.014202 0.066526 ( 0.000011 0.000014 0.000012 ) M - matrix: 0.004650 -0.000001 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000001 0.004625 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.004636 ( 0.000001 0.000001 0.000002 ) unit cell: 10.402(2) 10.430(2) 10.4172(19) 89.906(16) 90.015(17) 89.984(19) V = 1130.2(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066155 0.015271 0.006525 ( 0.000013 0.000018 0.000015 ) -0.016368 0.064790 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003344 -0.014170 0.066613 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004656 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004632 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066155 0.015271 0.006525 ( 0.000013 0.000018 0.000015 ) -0.016368 0.064790 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003344 -0.014170 0.066613 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.396(2) 10.422(2) 10.4041(18) 89.945(16) 89.960(15) 89.965(18) V = 1127.2(4) unit cell: 10.4073(5) 10.4073(5) 10.4073(5) 90.0 90.0 90.0 V = 1127.23(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.032) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066155 0.015271 0.006525 ( 0.000013 0.000018 0.000015 ) -0.016368 0.064790 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003344 -0.014170 0.066613 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004656 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004632 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066155 0.015271 0.006525 ( 0.000013 0.000018 0.000015 ) -0.016368 0.064790 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003344 -0.014170 0.066613 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.396(2) 10.422(2) 10.4041(18) 89.945(16) 89.960(15) 89.965(18) V = 1127.2(4) unit cell: 10.4073(5) 10.4073(5) 10.4073(5) 90.0 90.0 90.0 V = 1127.23(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068216 -0.000038 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068072 -0.000054 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068177 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004653 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004634 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068216 -0.000038 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068072 -0.000054 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068177 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.3979(16) 10.420(3) 10.4039(15) 89.964(16) 89.976(13) 89.968(17) V = 1127.2(4) unit cell: 10.4072(5) 10.4072(5) 10.4072(5) 90.0 90.0 90.0 V = 1127.20(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 266 obs out of 271 (total:271,skipped:0) (98.15%) UB - matrix: 0.065974 0.015323 0.006321 ( 0.000017 0.000012 0.000013 ) -0.016372 0.064790 0.013406 ( 0.000019 0.000014 0.000015 ) -0.002893 -0.014583 0.066492 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004629 -0.000008 0.000005 ( 0.000002 0.000002 0.000002 ) -0.000008 0.004645 -0.000004 ( 0.000002 0.000002 0.000001 ) 0.000005 -0.000004 0.004641 ( 0.000002 0.000001 0.000002 ) unit cell: 10.425(2) 10.407(2) 10.412(2) 89.948(17) 90.063(19) 89.906(19) V = 1129.7(4) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.066051 0.015388 0.006334 ( 0.000016 0.000012 0.000013 ) -0.016397 0.064849 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002877 -0.014635 0.066565 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004656 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004650 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066051 0.015388 0.006334 ( 0.000016 0.000012 0.000013 ) -0.016397 0.064849 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002877 -0.014635 0.066565 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.413(2) 10.395(2) 10.4018(18) 89.887(15) 90.093(17) 89.941(18) V = 1125.9(4) unit cell: 10.4032(5) 10.4032(5) 10.4032(5) 90.0 90.0 90.0 V = 1125.89(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.032) HKL list info: 1297 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066051 0.015388 0.006334 ( 0.000016 0.000012 0.000013 ) -0.016397 0.064849 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002877 -0.014635 0.066565 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004656 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004650 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066051 0.015388 0.006334 ( 0.000016 0.000012 0.000013 ) -0.016397 0.064849 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002877 -0.014635 0.066565 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.413(2) 10.395(2) 10.4018(18) 89.887(15) 90.093(17) 89.941(18) V = 1125.9(4) unit cell: 10.4032(5) 10.4032(5) 10.4032(5) 90.0 90.0 90.0 V = 1125.89(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068121 -0.000095 0.000071 ( 0.000017 0.000013 0.000014 ) 0.000059 0.068206 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068183 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004652 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068121 -0.000095 0.000071 ( 0.000017 0.000013 0.000014 ) 0.000059 0.068206 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068183 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.412(3) 10.3993(16) 10.4029(18) 89.931(13) 90.044(17) 89.971(16) V = 1126.4(4) unit cell: 10.4048(5) 10.4048(5) 10.4048(5) 90.0 90.0 90.0 V = 1126.43(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 181 obs out of 190 (total:190,skipped:0) (95.26%) UB - matrix: 0.066064 0.015589 0.006259 ( 0.000020 0.000017 0.000019 ) -0.016427 0.064833 0.013091 ( 0.000027 0.000023 0.000026 ) -0.003002 -0.014216 0.066512 ( 0.000034 0.000029 0.000033 ) M - matrix: 0.004643 0.000008 -0.000001 ( 0.000003 0.000002 0.000003 ) 0.000008 0.004648 0.000001 ( 0.000002 0.000003 0.000003 ) -0.000001 0.000001 0.004634 ( 0.000003 0.000003 0.000004 ) unit cell: 10.409(3) 10.403(4) 10.419(5) 90.01(3) 89.98(3) 90.09(3) V = 1128.3(7) OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 No constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004638 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.415(3) 10.421(3) 10.405(2) 89.85(2) 90.17(2) 90.10(2) V = 1129.2(5) unit cell: 10.4134(7) 10.4134(7) 10.4134(7) 90.0 90.0 90.0 V = 1129.23(13) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) HKL list info: 1265 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004638 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.415(3) 10.421(3) 10.405(2) 89.85(2) 90.17(2) 90.10(2) V = 1129.2(5) unit cell: 10.4134(7) 10.4134(7) 10.4134(7) 90.0 90.0 90.0 V = 1129.23(13) 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! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: 0.068131 0.000083 0.000194 ( 0.000020 0.000016 0.000019 ) -0.000013 0.068074 -0.000160 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068166 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000005 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000005 0.004634 -0.000011 ( 0.000002 0.000002 0.000002 ) 0.000013 -0.000011 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.068131 0.000083 0.000194 ( 0.000020 0.000016 0.000019 ) -0.000013 0.068074 -0.000160 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068166 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.411(3) 10.420(3) 10.4055(18) 89.867(19) 90.161(19) 90.06(2) V = 1128.7(5) unit cell: 10.4120(7) 10.4120(7) 10.4120(7) 90.0 90.0 90.0 V = 1128.75(12) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.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= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 87 obs out of 101 (total:101,skipped:0) (86.14%) UB - matrix: 0.066045 0.015283 0.006191 ( 0.000104 0.000052 0.000050 ) -0.016527 0.064641 0.013405 ( 0.000051 0.000026 0.000025 ) -0.002725 -0.014428 0.066485 ( 0.000078 0.000039 0.000038 ) M - matrix: 0.004642 -0.000020 0.000006 ( 0.000014 0.000005 0.000006 ) -0.000020 0.004620 0.000002 ( 0.000005 0.000004 0.000003 ) 0.000006 0.000002 0.004638 ( 0.000006 0.000003 0.000005 ) unit cell: 10.410(15) 10.435(5) 10.415(6) 90.02(4) 90.08(7) 89.76(7) V = 1131(2) OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 No constraint UB - matrix: 0.066203 0.015411 0.005952 ( 0.000054 0.000029 0.000028 ) -0.016509 0.064721 0.013535 ( 0.000030 0.000016 0.000016 ) -0.002359 -0.014564 0.066550 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004661 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004638 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004648 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066203 0.015411 0.005952 ( 0.000054 0.000029 0.000028 ) -0.016509 0.064721 0.013535 ( 0.000030 0.000016 0.000016 ) -0.002359 -0.014564 0.066550 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.390(8) 10.415(3) 10.404(3) 89.98(2) 90.17(3) 89.83(4) V = 1125.8(10) unit cell: 10.4029(9) 10.4029(9) 10.4029(9) 90.0 90.0 90.0 V = 1125.79(18) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.032) HKL list info: 672 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066203 0.015411 0.005952 ( 0.000054 0.000029 0.000028 ) -0.016509 0.064721 0.013535 ( 0.000030 0.000016 0.000016 ) -0.002359 -0.014564 0.066550 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004661 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004638 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004648 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066203 0.015411 0.005952 ( 0.000054 0.000029 0.000028 ) -0.016509 0.064721 0.013535 ( 0.000030 0.000016 0.000016 ) -0.002359 -0.014564 0.066550 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.390(8) 10.415(3) 10.404(3) 89.98(2) 90.17(3) 89.83(4) V = 1125.8(10) unit cell: 10.4029(9) 10.4029(9) 10.4029(9) 90.0 90.0 90.0 V = 1125.79(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 7) ******* No constraint UB - matrix: 0.068277 -0.000193 0.000205 ( 0.000053 0.000028 0.000028 ) -0.000007 0.068106 -0.000019 ( 0.000031 0.000017 0.000016 ) 0.000000 -0.000002 0.068172 ( 0.000033 0.000018 0.000018 ) M - matrix: 0.004662 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004638 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000001 0.004647 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.068277 -0.000193 0.000205 ( 0.000053 0.000028 0.000028 ) -0.000007 0.068106 -0.000019 ( 0.000031 0.000017 0.000016 ) 0.000000 -0.000002 0.068172 ( 0.000033 0.000018 0.000018 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.389(8) 10.415(2) 10.405(3) 89.98(2) 90.17(4) 89.83(3) V = 1125.7(10) unit cell: 10.4026(10) 10.4026(10) 10.4026(10) 90.0 90.0 90.0 V = 1125.71(18) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 56.89 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb *** 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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_proffitpeak_8" UB fit with 97 obs out of 102 (total:102,skipped:0) (95.10%) UB - matrix: 0.065895 0.015529 0.006026 ( 0.000073 0.000041 0.000035 ) -0.016571 0.064754 0.013388 ( 0.000042 0.000024 0.000020 ) -0.002519 -0.014324 0.066517 ( 0.000067 0.000038 0.000032 ) M - matrix: 0.004623 -0.000014 0.000008 ( 0.000010 0.000004 0.000005 ) -0.000014 0.004639 0.000008 ( 0.000004 0.000003 0.000003 ) 0.000008 0.000008 0.004640 ( 0.000005 0.000003 0.000004 ) unit cell: 10.432(11) 10.414(4) 10.413(5) 90.10(4) 90.09(6) 89.83(5) V = 1131(1) OTKP changes: 102 1 1 1 OTKP changes: 102 1 1 1 OTKP changes: 102 1 1 1 No constraint UB - matrix: 0.066024 0.015517 0.005975 ( 0.000049 0.000026 0.000023 ) -0.016521 0.064838 0.013407 ( 0.000039 0.000021 0.000019 ) -0.002453 -0.014525 0.066536 ( 0.000028 0.000015 0.000013 ) M - matrix: 0.004638 -0.000011 0.000010 ( 0.000007 0.000003 0.000002 ) -0.000011 0.004656 -0.000004 ( 0.000003 0.000003 0.000002 ) 0.000010 -0.000004 0.004642 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066024 0.015517 0.005975 ( 0.000049 0.000026 0.000023 ) -0.016521 0.064838 0.013407 ( 0.000039 0.000021 0.000019 ) -0.002453 -0.014525 0.066536 ( 0.000028 0.000015 0.000013 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 102 obs out of 102 (total:102,skipped:0) (100.00%) unit cell: 10.415(7) 10.395(4) 10.410(2) 89.95(2) 90.12(3) 89.86(4) V = 1127.1(9) unit cell: 10.4068(9) 10.4068(9) 10.4068(9) 90.0 90.0 90.0 V = 1127.08(18) Run 8 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.032) HKL list info: 717 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066024 0.015517 0.005975 ( 0.000049 0.000026 0.000023 ) -0.016521 0.064838 0.013407 ( 0.000039 0.000021 0.000019 ) -0.002453 -0.014525 0.066536 ( 0.000028 0.000015 0.000013 ) M - matrix: 0.004638 -0.000011 0.000010 ( 0.000007 0.000003 0.000002 ) -0.000011 0.004656 -0.000004 ( 0.000003 0.000003 0.000002 ) 0.000010 -0.000004 0.004642 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066024 0.015517 0.005975 ( 0.000049 0.000026 0.000023 ) -0.016521 0.064838 0.013407 ( 0.000039 0.000021 0.000019 ) -0.002453 -0.014525 0.066536 ( 0.000028 0.000015 0.000013 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 102 obs out of 102 (total:102,skipped:0) (100.00%) unit cell: 10.415(7) 10.395(4) 10.410(2) 89.95(2) 90.12(3) 89.86(4) V = 1127.1(9) unit cell: 10.4068(9) 10.4068(9) 10.4068(9) 90.0 90.0 90.0 V = 1127.08(18) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 102 obs out of 102 (total:102,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: 0.068102 -0.000156 0.000143 ( 0.000052 0.000028 0.000025 ) -0.000005 0.068233 -0.000061 ( 0.000033 0.000018 0.000016 ) 0.000002 -0.000004 0.068135 ( 0.000030 0.000016 0.000014 ) M - matrix: 0.004638 -0.000011 0.000010 ( 0.000007 0.000003 0.000003 ) -0.000011 0.004656 -0.000004 ( 0.000003 0.000002 0.000002 ) 0.000010 -0.000004 0.004642 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.068102 -0.000156 0.000143 ( 0.000052 0.000028 0.000025 ) -0.000005 0.068233 -0.000061 ( 0.000033 0.000018 0.000016 ) 0.000002 -0.000004 0.068135 ( 0.000030 0.000016 0.000014 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000001 ) UB fit with 102 obs out of 102 (total:102,skipped:0) (100.00%) unit cell: 10.415(8) 10.395(3) 10.410(2) 89.945(19) 90.12(3) 89.86(4) V = 1127.1(9) unit cell: 10.4070(9) 10.4070(9) 10.4070(9) 90.0 90.0 90.0 V = 1127.13(18) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_26.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068157 -0.000005 -0.000023 ( 0.000008 0.000008 0.000008 ) -0.000004 0.068103 0.000000 ( 0.000009 0.000008 0.000008 ) 0.000027 -0.000017 0.068174 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004645 -0.000001 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000001 0.004638 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000001 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068157 -0.000005 -0.000023 ( 0.000008 0.000008 0.000008 ) -0.000004 0.068103 0.000000 ( 0.000009 0.000008 0.000008 ) 0.000027 -0.000017 0.068174 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 1574 obs out of 1598 (total:1598,skipped:0) (98.50%) unit cell: 10.4069(13) 10.4151(13) 10.4043(9) 89.986(9) 90.003(9) 89.993(10) V = 1127.7(2) unit cell: 10.4088(3) 10.4088(3) 10.4088(3) 90.0 90.0 90.0 V = 1127.71(5) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 201 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_7.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_8.rrpprof 7066 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 15:12:40 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.032) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.032) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.032) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.032) Run 8 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.032) PROFFIT INFO: signal sum: min=-775.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-736.9381 max=1266349.7687 PROFFIT INFO: background sum: min=-93.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=423.0000 max=5775.0000 PROFFIT INFO: num of signal pixels: min=41 max=516 PROFFIT INFO: Inet: min=-1179.1011 max=2026159.6250 PROFFIT INFO: sig(Inet): min=52.0532 max=30723.5996 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=276.03 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 622 2407 3667 4384 4725 5496 5968 6252 6696 6992 7066 Percent 8.8 34.1 51.9 62.0 66.9 77.8 84.5 88.5 94.8 99.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 7066 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 7066 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2026160- 131223 706 413063.84 77.52 100.00 131070- 4043 706 29001.49 19.43 100.00 4035- 2113 706 2900.96 6.97 97.17 2110- 1247 706 1609.34 3.97 52.69 1246- 820 706 1019.29 2.34 15.86 820- 547 706 677.95 1.72 8.07 547- 344 706 442.56 1.24 5.24 343- 156 706 248.07 0.73 0.85 156- 19 706 82.69 0.30 0.00 19- -1179 712 -142.49 -0.28 0.00 ------------------------------------------------------------------------------------ 2026160- -1179 7066 44852.13 11.38 37.96 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 706 109612.17 15.57 67.85 1.64- 1.26 706 88087.30 21.46 57.93 1.26- 1.06 706 69039.52 20.39 70.40 1.06- 0.96 706 45627.41 12.73 31.16 0.96- 0.88 706 24695.62 8.96 46.32 0.88- 0.80 706 43300.42 12.26 34.42 0.80- 0.75 706 19688.09 6.07 20.25 0.75- 0.71 706 20427.56 6.67 16.15 0.71- 0.67 706 24807.28 8.04 28.75 0.67- 0.63 712 3586.65 1.78 6.60 ------------------------------------------------------------------------------------ 6.00- 0.63 7066 44852.13 11.38 37.96 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 15:12:40 2019 Sorting 7066 observations 53 unique observations with > 7.00 F2/sig(F2) 7066 observations in 8 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 8 0 49 711 Total number of frames 711 Maximum number of 53 frame scales suggested for reliable scaling Glued frame scales: 14 frame = 1 scale 7066 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 3 52 8 0 3 56 Total number of frames 56 1704 observations > 7.00 F2/sig(F2) 1704 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 6 47 7 0 3 51 8 0 3 55 Total number of frames 55 Removing 'redundancy=1' reflections Average redundancy: 24.2 (Out of 1704 removed 7 = 1697, 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): 2/m3bar 1697 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 6 47 7 0 3 51 8 0 3 55 Total number of frames 55 70 unique data precomputed (should be 70) 70 unique data with 1697 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 24.2 (Out of 1697 removed 0 = 1697, unique = 70) 70 unique data precomputed (should be 70) 70 unique data with 1697 observations RMS deviation of equivalent data = 0.30664 Rint = 0.24962 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24282, wR= 0.33300 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13385, wR= 0.18358, Acormin=0.469, Acormax=1.440, Acor_av=0.999 F test: Probability=1.000, F= 3.281 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13309, wR= 0.17831, Acormin=0.477, Acormax=1.482, Acor_av=0.985 F test: Probability=0.576, F= 1.010 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12619, wR= 0.17441, Acormin=0.556, Acormax=1.550, Acor_av=1.005 F test: Probability=0.988, F= 1.119 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12348, wR= 0.16698, Acormin=0.497, Acormax=1.570, Acor_av=0.994 F test: Probability=0.797, F= 1.042 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10464, wR= 0.14694, Acormin=0.557, Acormax=1.849, Acor_av=1.041 F test: Probability=1.000, F= 1.445 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11918, wR= 0.16649, Acormin=0.434, Acormax=1.642, Acor_av=0.987 F test: Probability=0.000, F= 0.769 Trying model 7 (ne=6, no=1)... Results: Rint= 0.11705, wR= 0.16045, Acormin=0.466, Acormax=1.634, Acor_av=0.983 F test: Probability=0.000, F= 0.796 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09912, wR= 0.14239, Acormin=0.534, Acormax=1.865, Acor_av=1.030 F test: Probability=0.977, F= 1.105 Trying model 9 (ne=6, no=5)... Results: Rint= 0.14334, wR= 0.18558, Acormin=0.130, Acormax=1.117, Acor_av=0.547 F test: Probability=0.000, F= 0.475 Final absorption model (ne=6, no=3): Rint= 0.09912, Acormin=0.534, Acormax=1.865, Acor_av=1.030 Combined refinement in use Rint: 0.25148 There are 55 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 91 pars with 4186 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30664 Using Levenberg-Marquardt: 0.00010 New wR= 0.10877 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24962 with corrections 0.08690 Rint for all data: 0.25148 with corrections 0.08956 4 observations identified as outliers and rejected Cycle 2 wR= 0.09685 Using Levenberg-Marquardt: 0.00001 New wR= 0.07972 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24971 with corrections 0.05953 Rint for all data: 0.25148 with corrections 0.06543 1 observations identified as outliers and rejected Cycle 3 wR= 0.07845 Using Levenberg-Marquardt: 0.00000 New wR= 0.07618 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24958 with corrections 0.05785 Rint for all data: 0.25148 with corrections 0.06480 0 observations identified as outliers and rejected Cycle 4 wR= 0.07618 Using Levenberg-Marquardt: 0.00000 New wR= 0.07544 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24958 with corrections 0.05723 Rint for all data: 0.25148 with corrections 0.06432 0 observations identified as outliers and rejected Cycle 5 wR= 0.07544 Using Levenberg-Marquardt: 0.00000 New wR= 0.07493 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24958 with corrections 0.05694 Rint for all data: 0.25148 with corrections 0.06411 0 observations identified as outliers and rejected Final wR= 0.07493 Final frame scales: Min= 0.7636 Max= 1.2447 Final absorption correction factors: Amin= 0.2865 Amax= 1.6116 PROFFIT INFO: Inet (after scale3 abspack): min=-1188.7755 max=1309608.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.1166 max=24203.3770 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/104 7066 reflections read from tmp file 283 reflections are rejected (282 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 7 3 2 4 3 215 Initial Chi^2= 0.53223 Cycle 1, Chi^2= 1.01243 Current error model SIG(F2)^2 = 61.46*I_RAW + 11.95*I_BACK+(0.03648*)^2 Cycle 2, Chi^2= 1.01324 Current error model SIG(F2)^2 = 75.48*I_RAW + 8.55*I_BACK+(0.02954*)^2 Cycle 3, Chi^2= 1.00657 Current error model SIG(F2)^2 = 81.24*I_RAW + 7.35*I_BACK+(0.02778*)^2 Cycle 4, Chi^2= 1.00241 Current error model SIG(F2)^2 = 83.30*I_RAW + 6.96*I_BACK+(0.02736*)^2 Cycle 5, Chi^2= 1.00079 Current error model SIG(F2)^2 = 83.97*I_RAW + 6.84*I_BACK+(0.02725*)^2 Cycle 6, Chi^2= 1.00025 Current error model SIG(F2)^2 = 84.18*I_RAW + 6.80*I_BACK+(0.02721*)^2 Cycle 7, Chi^2= 1.00008 Current error model SIG(F2)^2 = 84.25*I_RAW + 6.79*I_BACK+(0.02720*)^2 Final Chi^2= 1.00008 Final error model SIG(F2)^2 = 84.25*I_RAW + 6.79*I_BACK+(0.02720*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1309608- 117566 706 381215.74 30.03 100.00 116948- 3485 706 28957.49 12.99 100.00 3471- 2028 706 2694.87 6.18 99.43 2022- 1170 706 1517.37 3.97 68.13 1170- 777 706 956.82 2.80 27.48 777- 521 706 642.91 2.38 15.16 521- 330 706 420.13 1.97 8.78 329- 154 706 242.52 1.46 3.40 154- 20 706 81.49 0.72 0.14 20- -1189 712 -140.81 -0.57 0.00 ------------------------------------------------------------------------------------ 1309608- -1189 7066 41623.36 6.19 42.22 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 706 104163.09 10.04 71.67 1.64- 1.26 706 82188.74 9.29 61.19 1.26- 1.06 706 63275.57 8.84 74.65 1.06- 0.96 706 42312.34 5.79 33.99 0.96- 0.88 706 22803.58 5.61 54.11 0.88- 0.80 706 39676.98 6.58 41.50 0.80- 0.75 706 17979.20 3.98 23.23 0.75- 0.71 706 18389.07 4.69 20.54 0.71- 0.67 706 22363.12 5.39 33.00 0.67- 0.63 712 3406.68 1.69 8.57 ------------------------------------------------------------------------------------ 6.00- 0.63 7066 41623.36 6.19 42.22 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 706 104163.09 10.04 71.67 6.00- 1.26 1412 93175.91 9.67 66.43 6.00- 1.06 2118 83209.13 9.39 69.17 6.00- 0.96 2824 72984.93 8.49 60.38 6.00- 0.88 3530 62948.66 7.91 59.12 6.00- 0.80 4236 59070.05 7.69 56.19 6.00- 0.75 4942 53199.93 7.16 51.48 6.00- 0.71 5648 48848.57 6.85 47.61 6.00- 0.67 6354 45905.74 6.69 45.99 6.00- 0.63 7066 41623.36 6.19 42.22 ------------------------------------------------------------------------------------ 6.00- 0.63 7066 41623.36 6.19 42.22 Scale applied to data: s=0.763586 (maximum obs:1309608.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.064; Rsigma 0.038: data 7066 -> merged 240 With outlier rejection... Rint 0.054; Rsigma 0.039: data 7045 -> merged 240 Rejected total: 21, method kkm 10, method Blessing 11 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626534, 6.009508 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.42 - 1.59 21 21 37.81 100.00 794 1.57 - 1.20 21 21 39.76 100.00 835 1.19 - 1.02 21 21 37.48 100.00 787 1.02 - 0.91 21 21 36.38 100.00 764 0.91 - 0.84 21 21 32.10 100.00 674 0.84 - 0.78 21 21 31.43 100.00 660 0.78 - 0.74 21 21 29.62 100.00 622 0.74 - 0.71 21 21 25.19 100.00 529 0.71 - 0.68 21 21 27.76 100.00 583 0.68 - 0.65 23 23 23.70 100.00 545 --------------------------------------------------------------- 10.42 - 0.65 212 212 32.04 100.00 6793 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 15:12:41 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.406928 10.415135 10.404257 89.9863 90.0034 89.9932 7045 Reflections read from file xs2212a.hkl 7001 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.15 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3513 0 4644 4632 7001 N (int>3sigma) = 0 0 0 0 1587 0 2079 2046 2963 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.0 30.5 31.1 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.2 6.2 Lattice type: F chosen Volume: 1127.71 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 0.5000 Unitcell: 7.358 7.358 7.360 119.98 119.97 90.01 Niggli form: a.a = 54.135 b.b = 54.141 c.c = 54.168 b.c = -27.060 a.c = -27.051 a.b = -0.014 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.085 CUBIC F-lattice R(int) = 0.054 [ 6770] Vol = 1127.7 Cell: 10.415 10.407 10.404 90.00 90.01 89.99 Volume: 1127.71 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.035 TETRAGONAL I-lattice R(int) = 0.054 [ 6384] Vol = 563.9 Cell: 7.361 7.362 10.404 89.99 89.99 89.95 Volume: 563.86 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.024 TETRAGONAL I-lattice R(int) = 0.054 [ 6384] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 89.99 90.01 Volume: 563.86 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.066 TETRAGONAL I-lattice R(int) = 0.054 [ 6384] Vol = 563.9 Cell: 7.362 7.361 10.404 90.01 89.99 90.05 Volume: 563.86 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.011 ORTHORHOMBIC F-lattice R(int) = 0.053 [ 6331] Vol = 1127.7 Cell: 10.404 10.407 10.415 89.99 90.01 90.00 Volume: 1127.71 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.045 ORTHORHOMBIC I-lattice R(int) = 0.053 [ 6312] Vol = 563.9 Cell: 10.404 7.362 7.361 89.95 89.99 89.99 Volume: 563.86 Matrix: 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.024 ORTHORHOMBIC I-lattice R(int) = 0.052 [ 6311] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 90.01 90.01 Volume: 563.86 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.016 MONOCLINIC I-lattice R(int) = 0.051 [ 5785] Vol = 563.9 Cell: 7.361 10.404 7.362 89.99 90.05 90.01 Volume: 563.86 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.010 MONOCLINIC I-lattice R(int) = 0.052 [ 5783] Vol = 563.9 Cell: 7.360 10.407 7.362 90.00 90.06 89.99 Volume: 563.86 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) = 0.051 [ 5785] Vol = 563.9 Cell: 7.362 10.404 7.361 90.01 90.05 89.99 Volume: 563.86 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.022 MONOCLINIC I-lattice R(int) = 0.051 [ 5768] Vol = 563.9 Cell: 7.358 7.358 10.415 89.99 90.00 89.99 Volume: 563.86 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.017 MONOCLINIC I-lattice R(int) = 0.050 [ 5763] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 90.01 89.99 Volume: 563.86 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) = 0.050 [ 5783] Vol = 563.9 Cell: 7.358 10.415 7.358 90.00 90.01 89.99 Volume: 563.86 Matrix: 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.030 MONOCLINIC I-lattice R(int) = 0.050 [ 5783] Vol = 563.9 Cell: 7.358 10.415 7.358 90.00 90.01 90.01 Volume: 563.86 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) = 0.047 [ 4716] Vol = 281.9 Cell: 7.358 7.358 7.360 119.98 119.97 90.01 Volume: 281.93 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 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 3513 0 4644 4632 7001 N (int>3sigma) = 0 0 0 0 1587 0 2079 2046 2963 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.0 30.5 31.1 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.2 6.2 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.458 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 52 52 529 1374 N I>3s 2 2 2 736 0.0 0.0 -0.0 1.9 0.8 0.8 0.2 5.0 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 0.054 6269 Fd-3m 1 1 227 C N N N N 37 2284 0.055 6331 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415135 10.406928 10.404257 89.9966 90.0137 89.9932 ZERR 5.00 0.001278 0.001289 0.000945 0.0088 0.0088 0.0100 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1120203- 126232 700 685 26 26.3 378190.05 29.90 0.050 0.065 109027- 3176 796 793 26 30.5 26944.32 12.27 0.068 0.075 3018- 1411 1021 1019 26 39.2 2240.49 5.61 0.133 0.190 1331- 857 889 889 26 34.2 1059.05 2.80 0.232 0.302 845- 518 855 855 26 32.9 650.20 2.33 0.310 0.417 514- 306 896 896 26 34.5 392.02 1.79 0.420 0.578 302- 142 647 647 26 24.9 218.98 1.24 0.612 1.107 135- 23 624 623 26 24.0 69.81 0.53 0.890 2.627 19- -206 638 638 32 19.9 -26.72 -0.06 0.990 4.532 ------------------------------------------------------------------------------------------- 1120203- -206 7066 7045 240 29.4 40415.45 6.12 0.054 0.070 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-1.44 1023 1016 26 39.1 115194.89 11.04 0.051 0.065 0.030 1.39-1.09 1081 1077 26 41.4 42187.11 7.21 0.047 0.063 0.036 1.06-0.94 902 901 26 34.7 39201.06 5.60 0.051 0.062 0.037 0.92-0.84 859 858 26 33.0 41298.25 7.36 0.056 0.078 0.042 0.84-0.78 835 833 26 32.0 24132.89 4.91 0.060 0.078 0.048 0.78-0.73 710 708 26 27.2 8422.90 3.06 0.083 0.092 0.076 0.73-0.69 716 715 26 27.5 19639.68 4.78 0.067 0.080 0.061 0.69-0.66 679 678 28 24.2 13766.59 3.68 0.081 0.109 0.069 0.65-0.63 261 259 30 8.6 7942.33 2.34 0.080 0.073 0.087 ------------------------------------------------------------------------------------------------------ inf-0.63 7066 7045 240 29.4 40415.45 6.12 0.054 0.070 0.039 inf-0.65 6810 6791 211 32.2 41694.39 6.27 0.054 0.070 0.038 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-1.44 1016 26 26 100.0 39.1 115194.89 69.77 0.051 0.006 1.39-1.09 1077 26 26 100.0 41.4 42187.11 42.48 0.047 0.007 1.06-0.94 901 26 26 100.0 34.7 39201.06 34.29 0.051 0.007 0.92-0.84 858 26 26 100.0 33.0 41298.25 41.84 0.056 0.008 0.84-0.78 833 26 26 100.0 32.0 24132.89 26.55 0.060 0.009 0.78-0.73 708 26 26 100.0 27.2 8422.90 16.16 0.083 0.016 0.73-0.69 715 26 26 100.0 27.5 19639.68 23.89 0.067 0.012 0.69-0.66 678 28 28 100.0 24.2 13766.59 19.51 0.081 0.014 0.65-0.63 259 30 30 100.0 8.6 7942.33 6.62 0.080 0.033 -------------------------------------------------------------------------------------------- inf-0.63 7045 240 240 100.0 29.4 40415.45 35.35 0.054 0.008 inf-0.65 6791 211 211 100.0 32.2 41694.39 36.45 0.054 0.008 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066107 0.015170 0.006669 ( 0.000008 0.000008 0.000008 ) -0.016235 0.064802 0.013239 ( 0.000009 0.000008 0.000009 ) -0.003390 -0.014430 0.066543 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004645 -0.000000 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000000 0.004638 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000001 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066107 0.015170 0.006669 ( 0.000008 0.000008 0.000008 ) -0.016235 0.064802 0.013239 ( 0.000009 0.000008 0.000009 ) -0.003390 -0.014430 0.066543 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4070(13) 10.4155(13) 10.4043(9) 89.986(9) 90.004(9) 89.996(10) V = 1127.8(2) unit cell: 10.4090(3) 10.4090(3) 10.4090(3) 90.0 90.0 90.0 V = 1127.77(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.032) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.032) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.032) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.032) Run 8 Omega scan: (-49.000 - 1.000,50 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.032) PROFFIT INFO: signal sum: min=-775.0000 max=7910326.0000 PROFFIT INFO: signal sum lp corr: min=-736.9381 max=1266349.7687 PROFFIT INFO: background sum: min=-93.0000 max=8145.0000 PROFFIT INFO: background sum sig2: min=423.0000 max=5775.0000 PROFFIT INFO: num of signal pixels: min=41 max=516 PROFFIT INFO: Inet: min=-1179.1011 max=2026159.6250 PROFFIT INFO: sig(Inet): min=52.0532 max=30723.5996 PROFFIT INFO: Inet/sig(Inet): min=-2.10 max=276.03 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 1244 4814 7334 8768 9450 10992 11936 12504 13392 13984 14132 Percent 8.8 34.1 51.9 62.0 66.9 77.8 84.5 88.5 94.8 99.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 7066 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 7066 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2026160- 131223 706 413063.84 77.52 100.00 131070- 4043 706 29001.49 19.43 100.00 4035- 2113 706 2900.96 6.97 97.17 2110- 1247 706 1609.34 3.97 52.69 1246- 820 706 1019.29 2.34 15.86 820- 547 706 677.95 1.72 8.07 547- 344 706 442.56 1.24 5.24 343- 156 706 248.07 0.73 0.85 156- 19 706 82.69 0.30 0.00 19- -1179 712 -142.49 -0.28 0.00 ------------------------------------------------------------------------------------ 2026160- -1179 7066 44852.13 11.38 37.96 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 706 109612.17 15.57 67.85 1.64- 1.26 706 88087.30 21.46 57.93 1.26- 1.06 706 69039.52 20.39 70.40 1.06- 0.96 706 45627.41 12.73 31.16 0.96- 0.88 706 24695.62 8.96 46.32 0.88- 0.80 706 43300.42 12.26 34.42 0.80- 0.75 706 19688.09 6.07 20.25 0.75- 0.71 706 20427.56 6.67 16.15 0.71- 0.67 706 24807.28 8.04 28.75 0.67- 0.63 712 3586.65 1.78 6.60 ------------------------------------------------------------------------------------ 6.00- 0.63 7066 44852.13 11.38 37.96 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 15:12:42 2019 Sorting 7066 observations 43 unique observations with > 7.00 F2/sig(F2) 7066 observations in 8 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 8 0 49 711 Total number of frames 711 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 17 frame = 1 scale 7066 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 5 20 4 0 6 27 5 0 6 34 6 0 5 40 7 0 2 43 8 0 2 46 Total number of frames 46 1704 observations > 7.00 F2/sig(F2) 1704 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 5 13 3 0 5 19 4 0 6 26 5 0 6 33 6 0 5 39 7 0 2 42 8 0 2 45 Total number of frames 45 Removing 'redundancy=1' reflections Average redundancy: 30.4 (Out of 1704 removed 4 = 1700, unique = 56) 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 1700 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 5 13 3 0 5 19 4 0 6 26 5 0 6 33 6 0 5 39 7 0 2 42 8 0 2 45 Total number of frames 45 56 unique data precomputed (should be 56) 56 unique data with 1700 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 30.4 (Out of 1700 removed 0 = 1700, unique = 56) 56 unique data precomputed (should be 56) 56 unique data with 1700 observations RMS deviation of equivalent data = 0.30694 Rint = 0.24990 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24311, wR= 0.33329 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13386, wR= 0.18425, Acormin=0.470, Acormax=1.440, Acor_av=0.999 F test: Probability=1.000, F= 3.288 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13307, wR= 0.17903, Acormin=0.478, Acormax=1.481, Acor_av=0.985 F test: Probability=0.579, F= 1.010 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12598, wR= 0.17542, Acormin=0.557, Acormax=1.550, Acor_av=1.006 F test: Probability=0.990, F= 1.123 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12362, wR= 0.16786, Acormin=0.501, Acormax=1.570, Acor_av=0.995 F test: Probability=0.766, F= 1.037 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10471, wR= 0.14760, Acormin=0.559, Acormax=1.851, Acor_av=1.041 F test: Probability=1.000, F= 1.439 Final absorption model (ne=4, no=3): Rint= 0.10471, Acormin=0.559, Acormax=1.851, Acor_av=1.041 Combined refinement in use Rint: 0.25178 There are 45 active scales (one needs to be fixed) Refinement control: frame scale #30 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 68 pars with 2346 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30694 Using Levenberg-Marquardt: 0.00010 New wR= 0.11585 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24990 with corrections 0.08689 Rint for all data: 0.25178 with corrections 0.08957 2 observations identified as outliers and rejected Cycle 2 wR= 0.10950 Using Levenberg-Marquardt: 0.00001 New wR= 0.08811 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.25010 with corrections 0.06150 Rint for all data: 0.25178 with corrections 0.06592 0 observations identified as outliers and rejected Cycle 3 wR= 0.08811 Using Levenberg-Marquardt: 0.00000 New wR= 0.08346 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.25010 with corrections 0.05830 Rint for all data: 0.25178 with corrections 0.06270 0 observations identified as outliers and rejected Cycle 4 wR= 0.08346 Using Levenberg-Marquardt: 0.00000 New wR= 0.08141 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.25010 with corrections 0.05686 Rint for all data: 0.25178 with corrections 0.06120 0 observations identified as outliers and rejected Cycle 5 wR= 0.08141 Using Levenberg-Marquardt: 0.00000 New wR= 0.08025 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.25010 with corrections 0.05608 Rint for all data: 0.25178 with corrections 0.06035 0 observations identified as outliers and rejected Final wR= 0.08025 Final frame scales: Min= 0.6539 Max= 1.1285 Final absorption correction factors: Amin= 0.3949 Amax= 1.5008 PROFFIT INFO: Inet (after scale3 abspack): min=-1146.3403 max=1279042.3750 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=38.7956 max=23023.1602 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/104 7066 reflections read from tmp file 304 reflections are rejected (304 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 1 1 3 0 5 2 0 150 Initial Chi^2= 0.52156 Cycle 1, Chi^2= 1.00489 Current error model SIG(F2)^2 = 60.04*I_RAW + 12.45*I_BACK+(0.03718*)^2 Cycle 2, Chi^2= 1.00980 Current error model SIG(F2)^2 = 73.85*I_RAW + 9.13*I_BACK+(0.02979*)^2 Cycle 3, Chi^2= 1.00595 Current error model SIG(F2)^2 = 80.04*I_RAW + 7.83*I_BACK+(0.02750*)^2 Cycle 4, Chi^2= 1.00236 Current error model SIG(F2)^2 = 82.38*I_RAW + 7.38*I_BACK+(0.02685*)^2 Cycle 5, Chi^2= 1.00077 Current error model SIG(F2)^2 = 83.14*I_RAW + 7.25*I_BACK+(0.02668*)^2 Cycle 6, Chi^2= 1.00024 Current error model SIG(F2)^2 = 83.38*I_RAW + 7.20*I_BACK+(0.02663*)^2 Cycle 7, Chi^2= 1.00007 Current error model SIG(F2)^2 = 83.45*I_RAW + 7.19*I_BACK+(0.02661*)^2 Final Chi^2= 1.00007 Final error model SIG(F2)^2 = 83.45*I_RAW + 7.19*I_BACK+(0.02661*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1279042- 118091 706 379676.72 30.53 100.00 117707- 3484 706 28991.30 13.08 100.00 3478- 2015 706 2691.52 6.22 99.29 2015- 1168 706 1523.32 3.97 68.56 1167- 780 706 955.32 2.80 27.76 779- 522 706 644.83 2.40 15.44 522- 333 706 421.12 1.95 8.36 332- 155 706 242.45 1.46 3.40 154- 20 706 81.30 0.72 0.28 20- -1146 712 -141.77 -0.57 0.00 ------------------------------------------------------------------------------------ 1279042- -1146 7066 41473.24 6.25 42.27 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 706 103442.00 10.15 71.67 1.64- 1.26 706 81037.73 9.40 61.33 1.26- 1.06 706 63202.69 8.95 74.79 1.06- 0.96 706 42430.89 5.86 33.99 0.96- 0.88 706 22864.19 5.65 54.11 0.88- 0.80 706 39650.84 6.67 41.64 0.80- 0.75 706 18152.47 4.01 23.23 0.75- 0.71 706 18464.65 4.73 20.68 0.71- 0.67 706 22444.35 5.44 33.00 0.67- 0.63 712 3366.49 1.69 8.57 ------------------------------------------------------------------------------------ 6.00- 0.63 7066 41473.24 6.25 42.27 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 706 103442.00 10.15 71.67 6.00- 1.26 1412 92239.86 9.77 66.50 6.00- 1.06 2118 82560.81 9.50 69.26 6.00- 0.96 2824 72528.33 8.59 60.45 6.00- 0.88 3530 62595.50 8.00 59.18 6.00- 0.80 4236 58771.39 7.78 56.26 6.00- 0.75 4942 52968.69 7.24 51.54 6.00- 0.71 5648 48655.68 6.93 47.68 6.00- 0.67 6354 45743.31 6.76 46.05 6.00- 0.63 7066 41473.24 6.25 42.27 ------------------------------------------------------------------------------------ 6.00- 0.63 7066 41473.24 6.25 42.27 Scale applied to data: s=0.781834 (maximum obs:1279042.375,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.060; Rsigma 0.038: data 7066 -> merged 162 With outlier rejection... Rint 0.054; Rsigma 0.038: data 7048 -> merged 162 Rejected total: 18, method kkm 3, method Blessing 15 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.626545, 6.009612 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.42 - 1.76 14 14 45.57 100.00 638 1.73 - 1.27 14 14 49.93 100.00 699 1.26 - 1.06 14 14 57.07 100.00 799 1.05 - 0.97 14 14 49.43 100.00 692 0.95 - 0.88 14 14 52.07 100.00 729 0.87 - 0.81 14 14 46.50 100.00 651 0.80 - 0.76 14 14 48.79 100.00 683 0.76 - 0.72 14 14 40.14 100.00 562 0.72 - 0.69 14 14 45.14 100.00 632 0.69 - 0.65 19 19 37.37 100.00 710 --------------------------------------------------------------- 10.42 - 0.65 145 145 46.86 100.00 6795 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 15:12:41 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.406928 10.415135 10.404257 89.9863 90.0034 89.9932 7045 Reflections read from file xs2212a.hkl 7001 Reflections used for space-group determination (up to diffraction limit of 0.63A); mean (I/sigma) = 6.15 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3513 0 4644 4632 7001 N (int>3sigma) = 0 0 0 0 1587 0 2079 2046 2963 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.0 30.5 31.1 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.2 6.2 Lattice type: F chosen Volume: 1127.71 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 0.5000 Unitcell: 7.358 7.358 7.360 119.98 119.97 90.01 Niggli form: a.a = 54.135 b.b = 54.141 c.c = 54.168 b.c = -27.060 a.c = -27.051 a.b = -0.014 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.085 CUBIC F-lattice R(int) = 0.054 [ 6770] Vol = 1127.7 Cell: 10.415 10.407 10.404 90.00 90.01 89.99 Volume: 1127.71 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.035 TETRAGONAL I-lattice R(int) = 0.054 [ 6384] Vol = 563.9 Cell: 7.361 7.362 10.404 89.99 89.99 89.95 Volume: 563.86 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.024 TETRAGONAL I-lattice R(int) = 0.054 [ 6384] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 89.99 90.01 Volume: 563.86 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.066 TETRAGONAL I-lattice R(int) = 0.054 [ 6384] Vol = 563.9 Cell: 7.362 7.361 10.404 90.01 89.99 90.05 Volume: 563.86 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.011 ORTHORHOMBIC F-lattice R(int) = 0.053 [ 6331] Vol = 1127.7 Cell: 10.404 10.407 10.415 89.99 90.01 90.00 Volume: 1127.71 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.045 ORTHORHOMBIC I-lattice R(int) = 0.053 [ 6312] Vol = 563.9 Cell: 10.404 7.362 7.361 89.95 89.99 89.99 Volume: 563.86 Matrix: 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.024 ORTHORHOMBIC I-lattice R(int) = 0.052 [ 6311] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 90.01 90.01 Volume: 563.86 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.016 MONOCLINIC I-lattice R(int) = 0.051 [ 5785] Vol = 563.9 Cell: 7.361 10.404 7.362 89.99 90.05 90.01 Volume: 563.86 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.010 MONOCLINIC I-lattice R(int) = 0.052 [ 5783] Vol = 563.9 Cell: 7.360 10.407 7.362 90.00 90.06 89.99 Volume: 563.86 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) = 0.051 [ 5785] Vol = 563.9 Cell: 7.362 10.404 7.361 90.01 90.05 89.99 Volume: 563.86 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [37] err= 0.022 MONOCLINIC I-lattice R(int) = 0.051 [ 5768] Vol = 563.9 Cell: 7.358 7.358 10.415 89.99 90.00 89.99 Volume: 563.86 Matrix:-0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.017 MONOCLINIC I-lattice R(int) = 0.050 [ 5763] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 90.01 89.99 Volume: 563.86 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) = 0.050 [ 5783] Vol = 563.9 Cell: 7.358 10.415 7.358 90.00 90.01 89.99 Volume: 563.86 Matrix: 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.030 MONOCLINIC I-lattice R(int) = 0.050 [ 5783] Vol = 563.9 Cell: 7.358 10.415 7.358 90.00 90.01 90.01 Volume: 563.86 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) = 0.047 [ 4716] Vol = 281.9 Cell: 7.358 7.358 7.360 119.98 119.97 90.01 Volume: 281.93 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 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 3513 0 4644 4632 7001 N (int>3sigma) = 0 0 0 0 1587 0 2079 2046 2963 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 32.0 30.5 31.1 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.3 6.2 6.2 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.458 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 52 52 529 1374 N I>3s 2 2 2 736 0.0 0.0 -0.0 1.9 0.8 0.8 0.2 5.0 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 0.054 6269 Fd-3m 1 1 227 C N N N N 37 2284 0.055 6331 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415135 10.406928 10.404257 89.9966 90.0137 89.9932 ZERR 5.00 0.001278 0.001289 0.000945 0.0088 0.0088 0.0100 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1126390- 92903 855 842 27 31.2 330316.15 28.74 0.051 0.066 78794- 1778 1332 1330 27 49.3 5282.51 8.36 0.089 0.100 1761- 764 1428 1427 27 52.9 1133.24 3.02 0.226 0.299 762- 330 1393 1392 27 51.6 500.09 2.02 0.362 0.513 329- 82 995 995 27 36.9 210.08 1.16 0.626 1.228 62- -182 1063 1062 27 39.3 7.02 0.17 0.961 3.976 ------------------------------------------------------------------------------------------- 1126390- -182 7066 7048 162 43.5 40817.49 6.21 0.054 0.070 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-1.27 1340 1335 27 49.4 95116.32 10.16 0.049 0.063 0.030 1.26-0.97 1448 1443 27 53.4 50754.83 7.22 0.050 0.065 0.035 0.97-0.81 1401 1398 28 49.9 31266.32 6.17 0.059 0.078 0.043 0.81-0.73 1249 1247 28 44.5 17581.92 4.20 0.062 0.080 0.055 0.72-0.67 1082 1080 27 40.0 18117.19 4.59 0.077 0.100 0.063 0.66-0.63 546 545 25 21.8 4147.96 1.80 0.115 0.089 0.122 ------------------------------------------------------------------------------------------------------ inf-0.63 7066 7048 162 43.5 40817.49 6.21 0.054 0.070 0.038 inf-0.65 6810 6793 144 47.2 42108.17 6.37 0.054 0.069 0.038 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-1.27 1335 27 27 100.0 49.4 95116.32 68.91 0.049 0.006 1.26-0.97 1443 27 27 100.0 53.4 50754.83 49.74 0.050 0.006 0.97-0.81 1398 28 28 100.0 49.9 31266.32 43.40 0.059 0.008 0.81-0.73 1247 28 28 100.0 44.5 17581.92 25.59 0.062 0.010 0.72-0.67 1080 27 27 100.0 40.0 18117.19 30.81 0.077 0.010 0.66-0.63 545 25 25 100.0 21.8 4147.96 8.30 0.115 0.028 -------------------------------------------------------------------------------------------- inf-0.63 7048 162 162 100.0 43.5 40817.49 41.73 0.054 0.007 inf-0.65 6793 144 144 100.0 47.2 42108.17 43.04 0.054 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 15:18:56 2019) ID: 3668; threads 40; handles 809; mem 515872.00 (1204692.00)kB; time: 1w 5d 1h 29m 44s MEMORY INFO: Memory PF:231.0, Ph:563.0, V:1176.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:503.8,peak PF: 700.2, WS: 472.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:233.0, Ph:564.0, V:1178.0; MEMORY INFO: Process info - Handles: 810, Memory: PF:505.6,peak PF: 700.2, WS: 473.8, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 15:18:56 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000011 0.000012 0.000012 ) -0.015931 0.064696 0.013068 ( 0.000011 0.000011 0.000011 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000015 ) 10.42433 ( 0.00176 ) 10.43788 ( 0.00176 ) 10.40727 ( 0.00220 ) 89.88512 ( 0.01553 ) 89.79539 ( 0.01537 ) 90.20497 ( 0.01370 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\plots_red\xs2212a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs2212a\xs2212a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs2212a\xs2212a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs2212a\xs2212a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs2212a\xs2212a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs2212a\xs2212a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs2212a\xs2212a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs2212a\xs2212a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 15:18:56 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000011 0.000012 0.000012 ) -0.015931 0.064696 0.013068 ( 0.000011 0.000011 0.000011 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000015 0.000015 ) M - matrix: 0.004651 -0.000001 -0.000002 ( 0.000002 0.000001 0.000001 ) -0.000001 0.004640 -0.000001 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000001 0.004642 ( 0.000001 0.000001 0.000002 ) unit cell: 10.4243(18) 10.4379(18) 10.407(2) 89.885(16) 89.795(15) 90.205(14) V = 1132.4(4) unit cell: 10.4081(6) 10.4081(6) 10.4081(6) 90.0 90.0 90.0 V = 1127.50(11) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.938 ( 0.170) | 0.923 ( 0.398) | 1.01- 0.88 | 22 | 0.957 ( 0.073) | 1.004 ( 0.124) | 1.180 ( 0.493) | 0.88- 0.79 | 22 | 0.985 ( 0.059) | 1.028 ( 0.140) | 1.234 ( 0.387) | 0.79- 0.70 | 22 | 0.984 ( 0.041) | 0.962 ( 0.107) | 1.276 ( 0.475) | 0.70- 0.63 | 22 | 0.943 ( 0.038) | 0.917 ( 0.081) | 1.311 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 220 | 0.933 ( 0.193) | 0.943 ( 0.158) | 1.113 ( 0.914) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 251 peaks identified as outliers and rejected 251 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 251 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 251 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.933 ( 0.064) | 0.964 ( 0.109) | 0.868 ( 0.326) | 1.09- 0.91 | 25 | 0.958 ( 0.066) | 0.981 ( 0.099) | 1.061 ( 0.453) | 0.89- 0.82 | 25 | 0.934 ( 0.070) | 0.926 ( 0.093) | 1.119 ( 0.390) | 0.82- 0.72 | 25 | 0.952 ( 0.053) | 0.902 ( 0.085) | 1.407 ( 0.453) | 0.72- 0.63 | 26 | 0.928 ( 0.033) | 0.880 ( 0.090) | 1.365 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 251 | 0.920 ( 0.080) | 0.917 ( 0.119) | 1.055 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 251 obs out of 251 (total:251,skipped:0) (100.00%) UB - matrix: 0.066196 0.014133 0.006718 ( 0.000026 0.000034 0.000033 ) -0.015600 0.064667 0.012815 ( 0.000017 0.000022 0.000022 ) -0.003911 -0.014166 0.066843 ( 0.000023 0.000029 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004582 -0.000023 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000023 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.479(4) 10.371(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.6(7) OTKP changes: 251 1 1 1 OTKP changes: 251 1 1 1 No constraint UB - matrix: 0.066328 0.014183 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015580 0.064687 0.012854 ( 0.000017 0.000023 0.000022 ) -0.004072 -0.014197 0.066893 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004587 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066328 0.014183 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015580 0.064687 0.012854 ( 0.000017 0.000023 0.000022 ) -0.004072 -0.014197 0.066893 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 251 obs out of 251 (total:251,skipped:0) (100.00%) unit cell: 10.392(4) 10.473(3) 10.362(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.7(7) unit cell: 10.4088(5) 10.4088(5) 10.4088(5) 90.0 90.0 90.0 V = 1127.73(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.010) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066328 0.014183 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015580 0.064687 0.012854 ( 0.000017 0.000023 0.000022 ) -0.004072 -0.014197 0.066893 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004587 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066328 0.014183 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015580 0.064687 0.012854 ( 0.000017 0.000023 0.000022 ) -0.004072 -0.014197 0.066893 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 251 obs out of 251 (total:251,skipped:0) (100.00%) unit cell: 10.392(4) 10.473(3) 10.362(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.7(7) unit cell: 10.4088(5) 10.4088(5) 10.4088(5) 90.0 90.0 90.0 V = 1127.73(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 251 obs out of 251 (total:251,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 255 peaks identified as outliers and rejected 255 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 255 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 255 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 26 | 0.869 ( 0.088) | 0.876 ( 0.126) | 1.009 ( 0.497) | 2.37- 1.75 | 26 | 0.881 ( 0.097) | 0.900 ( 0.140) | 1.045 ( 0.533) | 1.75- 1.58 | 26 | 0.898 ( 0.094) | 0.880 ( 0.154) | 0.948 ( 0.391) | 1.58- 1.35 | 26 | 0.942 ( 0.084) | 0.962 ( 0.111) | 0.923 ( 0.446) | 1.35- 1.16 | 26 | 0.919 ( 0.075) | 0.921 ( 0.111) | 0.999 ( 0.581) | 1.16- 1.06 | 26 | 0.924 ( 0.071) | 0.963 ( 0.119) | 0.792 ( 0.261) | 1.06- 0.89 | 26 | 0.957 ( 0.065) | 0.970 ( 0.107) | 1.072 ( 0.459) | 0.89- 0.82 | 26 | 0.944 ( 0.071) | 0.928 ( 0.084) | 1.172 ( 0.407) | 0.79- 0.69 | 26 | 0.953 ( 0.048) | 0.916 ( 0.103) | 1.305 ( 0.463) | 0.69- 0.63 | 21 | 0.927 ( 0.036) | 0.869 ( 0.075) | 1.380 ( 0.452) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 255 | 0.921 ( 0.081) | 0.919 ( 0.121) | 1.058 ( 0.485) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 221 peaks identified as outliers and rejected 221 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 221 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 221 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.886 ( 0.167) | 0.784 ( 0.226) | 1.59- 1.36 | 22 | 0.961 ( 0.074) | 0.996 ( 0.118) | 0.881 ( 0.464) | 1.36- 1.19 | 22 | 0.929 ( 0.083) | 0.946 ( 0.101) | 0.892 ( 0.523) | 1.19- 1.01 | 22 | 0.967 ( 0.080) | 0.997 ( 0.117) | 0.860 ( 0.275) | 1.01- 0.88 | 22 | 0.980 ( 0.065) | 0.992 ( 0.077) | 1.016 ( 0.381) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.984 ( 0.130) | 1.003 ( 0.383) | 0.79- 0.69 | 22 | 0.965 ( 0.045) | 0.919 ( 0.090) | 1.202 ( 0.474) | 0.69- 0.63 | 23 | 0.933 ( 0.049) | 0.855 ( 0.074) | 1.289 ( 0.440) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 221 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.978 ( 0.429) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.156) HKL list info: 1283 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 192 peaks identified as outliers and rejected 192 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 192 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 192 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.97 | 19 | 0.842 ( 0.116) | 0.844 ( 0.171) | 0.956 ( 0.449) | 2.63- 1.84 | 19 | 0.822 ( 0.111) | 0.843 ( 0.187) | 0.847 ( 0.504) | 1.84- 1.59 | 19 | 0.842 ( 0.108) | 0.837 ( 0.164) | 0.836 ( 0.354) | 1.59- 1.36 | 19 | 0.936 ( 0.096) | 0.973 ( 0.144) | 0.805 ( 0.268) | 1.36- 1.20 | 19 | 0.950 ( 0.102) | 0.972 ( 0.160) | 0.845 ( 0.330) | 1.20- 1.01 | 19 | 0.995 ( 0.078) | 1.010 ( 0.137) | 1.101 ( 0.434) | 1.01- 0.88 | 19 | 0.998 ( 0.085) | 1.016 ( 0.121) | 1.030 ( 0.364) | 0.88- 0.79 | 19 | 1.037 ( 0.059) | 1.056 ( 0.123) | 0.938 ( 0.316) | 0.79- 0.72 | 19 | 1.031 ( 0.054) | 0.994 ( 0.144) | 1.279 ( 0.526) | 0.70- 0.63 | 21 | 0.975 ( 0.052) | 0.883 ( 0.059) | 1.164 ( 0.415) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 192 | 0.943 ( 0.117) | 0.942 ( 0.164) | 0.982 ( 0.432) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) UB - matrix: 0.065810 0.015591 0.006262 ( 0.000023 0.000019 0.000022 ) -0.016403 0.064531 0.013131 ( 0.000023 0.000020 0.000022 ) -0.002751 -0.014148 0.066421 ( 0.000026 0.000022 0.000025 ) M - matrix: 0.004608 0.000006 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004607 0.000005 ( 0.000002 0.000003 0.000002 ) 0.000014 0.000005 0.004623 ( 0.000002 0.000002 0.000003 ) unit cell: 10.450(3) 10.450(3) 10.432(4) 90.07(3) 90.17(3) 90.08(3) V = 1139.1(6) OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 1279 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 190 peaks identified as outliers and rejected 190 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 190 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 190 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 3.00 | 19 | 0.846 ( 0.114) | 0.847 ( 0.168) | 0.873 ( 0.501) | 2.99- 2.00 | 19 | 0.802 ( 0.108) | 0.800 ( 0.186) | 0.843 ( 0.452) | 1.84- 1.59 | 19 | 0.842 ( 0.097) | 0.828 ( 0.155) | 0.880 ( 0.351) | 1.59- 1.36 | 19 | 0.948 ( 0.083) | 0.983 ( 0.140) | 0.851 ( 0.258) | 1.36- 1.19 | 19 | 0.950 ( 0.094) | 0.960 ( 0.152) | 0.768 ( 0.211) | 1.19- 1.00 | 19 | 1.018 ( 0.060) | 1.041 ( 0.127) | 1.085 ( 0.364) | 1.00- 0.88 | 19 | 1.010 ( 0.085) | 1.031 ( 0.121) | 1.045 ( 0.373) | 0.88- 0.78 | 19 | 1.033 ( 0.056) | 1.044 ( 0.117) | 0.953 ( 0.322) | 0.78- 0.69 | 19 | 1.031 ( 0.055) | 1.004 ( 0.165) | 1.278 ( 0.531) | 0.69- 0.63 | 19 | 0.970 ( 0.050) | 0.876 ( 0.055) | 1.127 ( 0.364) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 190 | 0.945 ( 0.116) | 0.942 ( 0.169) | 0.970 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 UB - matrix: 0.066110 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) UB - matrix: 0.066109 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) 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= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 100 peaks identified as outliers and rejected 100 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 100 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 100 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 2.37 | 10 | 0.824 ( 0.107) | 0.789 ( 0.168) | 0.948 ( 0.526) | 2.13- 1.65 | 10 | 0.887 ( 0.099) | 0.902 ( 0.146) | 0.800 ( 0.370) | 1.64- 1.46 | 10 | 0.917 ( 0.142) | 0.896 ( 0.234) | 0.948 ( 0.416) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.161) | 1.038 ( 0.459) | 1.23- 1.11 | 10 | 1.014 ( 0.089) | 1.022 ( 0.172) | 1.004 ( 0.500) | 1.11- 1.00 | 10 | 0.988 ( 0.107) | 1.011 ( 0.206) | 0.971 ( 0.392) | 1.00- 0.89 | 10 | 1.016 ( 0.106) | 1.093 ( 0.173) | 0.829 ( 0.141) | 0.89- 0.86 | 10 | 0.995 ( 0.094) | 1.038 ( 0.093) | 1.245 ( 0.487) | 0.82- 0.73 | 10 | 1.072 ( 0.046) | 1.130 ( 0.142) | 0.868 ( 0.108) | 0.72- 0.64 | 10 | 1.031 ( 0.064) | 1.069 ( 0.171) | 1.233 ( 0.765) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 0.64 | 100 | 0.972 ( 0.121) | 0.995 ( 0.197) | 0.988 ( 0.476) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) UB - matrix: 0.065966 0.015448 0.005965 ( 0.000053 0.000028 0.000028 ) -0.016426 0.064502 0.013369 ( 0.000054 0.000029 0.000028 ) -0.002418 -0.014553 0.066425 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004627 -0.000005 0.000013 ( 0.000007 0.000004 0.000003 ) -0.000005 0.004611 -0.000012 ( 0.000004 0.000004 0.000002 ) 0.000013 -0.000012 0.004627 ( 0.000003 0.000002 0.000002 ) unit cell: 10.427(8) 10.446(5) 10.428(3) 89.85(3) 90.16(4) 89.93(5) V = 1136(1) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) 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! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 101 peaks identified as outliers and rejected 101 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 101 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 101 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.38 | 10 | 0.825 ( 0.107) | 0.790 ( 0.169) | 1.019 ( 0.527) | 2.13- 1.64 | 10 | 0.860 ( 0.122) | 0.859 ( 0.190) | 0.860 ( 0.389) | 1.64- 1.46 | 10 | 0.944 ( 0.113) | 0.943 ( 0.190) | 0.940 ( 0.402) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.160) | 1.023 ( 0.449) | 1.23- 1.11 | 10 | 1.002 ( 0.107) | 0.995 ( 0.210) | 0.997 ( 0.506) | 1.09- 1.00 | 10 | 1.034 ( 0.082) | 1.115 ( 0.140) | 0.886 ( 0.284) | 0.97- 0.88 | 10 | 0.989 ( 0.091) | 1.159 ( 0.229) | 0.740 ( 0.286) | 0.88- 0.86 | 10 | 1.009 ( 0.084) | 1.059 ( 0.096) | 1.119 ( 0.453) | 0.82- 0.73 | 10 | 1.071 ( 0.046) | 1.128 ( 0.142) | 0.868 ( 0.110) | 0.72- 0.63 | 11 | 1.023 ( 0.066) | 1.042 ( 0.168) | 1.108 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.63 | 101 | 0.974 ( 0.119) | 1.009 ( 0.206) | 0.958 ( 0.416) | 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_51.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_8_51.rpb PROFFITPEAK info: 301 peaks in the peak location table UB fit with 117 obs out of 178 (total:178,skipped:0) (65.73%) UB - matrix: 0.065892 0.015282 0.006429 ( 0.000092 0.000048 0.000050 ) -0.016535 0.064746 0.013323 ( 0.000074 0.000038 0.000040 ) -0.003162 -0.014322 0.066501 ( 0.000097 0.000051 0.000052 ) M - matrix: 0.004625 -0.000018 -0.000007 ( 0.000012 0.000006 0.000007 ) -0.000018 0.004631 0.000008 ( 0.000006 0.000005 0.000004 ) -0.000007 0.000008 0.004641 ( 0.000007 0.000004 0.000007 ) unit cell: 10.430(13) 10.423(7) 10.412(8) 90.10(6) 89.91(9) 89.77(8) V = 1132(2) UB fit with 117 obs out of 178 (total:178,skipped:0) (65.73%) UB - matrix: 0.065892 0.015282 0.006429 ( 0.000092 0.000048 0.000050 ) -0.016535 0.064746 0.013323 ( 0.000074 0.000038 0.000040 ) -0.003162 -0.014322 0.066501 ( 0.000097 0.000051 0.000052 ) M - matrix: 0.004625 -0.000018 -0.000007 ( 0.000012 0.000006 0.000007 ) -0.000018 0.004631 0.000008 ( 0.000006 0.000005 0.000004 ) -0.000007 0.000008 0.004641 ( 0.000007 0.000004 0.000007 ) unit cell: 10.430(13) 10.423(7) 10.412(8) 90.10(6) 89.91(9) 89.77(8) V = 1132(2) OTKP changes: 67 1 1 1 OTKP changes: 67 1 1 1 OTKP changes: 67 1 1 1 No constraint UB - matrix: 0.065734 0.015568 0.005983 ( 0.000062 0.000033 0.000040 ) -0.016533 0.064611 0.013441 ( 0.000041 0.000022 0.000027 ) -0.002363 -0.014557 0.066403 ( 0.000037 0.000020 0.000024 ) M - matrix: 0.004600 -0.000010 0.000014 ( 0.000008 0.000004 0.000004 ) -0.000010 0.004629 -0.000005 ( 0.000004 0.000003 0.000002 ) 0.000014 -0.000005 0.004626 ( 0.000004 0.000002 0.000003 ) Constraint UB - matrix: 0.065734 0.015568 0.005983 ( 0.000062 0.000033 0.000040 ) -0.016533 0.064611 0.013441 ( 0.000041 0.000022 0.000027 ) -0.002363 -0.014557 0.066403 ( 0.000037 0.000020 0.000024 ) M - matrix: 0.004621 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004621 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004621 ( 0.000000 0.000000 0.000001 ) UB fit with 167 obs out of 178 (total:178,skipped:0) (93.82%) unit cell: 10.458(9) 10.426(4) 10.429(4) 89.94(3) 90.18(4) 89.87(5) V = 1137(1) unit cell: 10.4375(16) 10.4375(16) 10.4375(16) 90.0 90.0 90.0 V = 1137.1(3) UB fit with 167 obs out of 178 (total:178,skipped:0) (93.82%) UB - matrix: 0.065734 0.015568 0.005983 ( 0.000062 0.000033 0.000040 ) -0.016533 0.064611 0.013441 ( 0.000041 0.000022 0.000027 ) -0.002363 -0.014557 0.066403 ( 0.000037 0.000020 0.000024 ) M - matrix: 0.004600 -0.000010 0.000014 ( 0.000008 0.000004 0.000004 ) -0.000010 0.004629 -0.000005 ( 0.000004 0.000003 0.000002 ) 0.000014 -0.000005 0.004626 ( 0.000004 0.000002 0.000003 ) unit cell: 10.458(9) 10.426(4) 10.429(4) 89.94(3) 90.18(4) 89.87(5) V = 1137(1) OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 OTKP changes: 68 1 1 1 178 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_8" Run 8 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.156) HKL list info: 1012 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065734 0.015568 0.005983 ( 0.000062 0.000033 0.000040 ) -0.016533 0.064611 0.013441 ( 0.000041 0.000022 0.000027 ) -0.002363 -0.014557 0.066403 ( 0.000037 0.000020 0.000024 ) M - matrix: 0.004600 -0.000010 0.000014 ( 0.000008 0.000004 0.000004 ) -0.000010 0.004629 -0.000005 ( 0.000004 0.000003 0.000002 ) 0.000014 -0.000005 0.004626 ( 0.000004 0.000002 0.000003 ) Constraint UB - matrix: 0.065734 0.015568 0.005983 ( 0.000062 0.000033 0.000040 ) -0.016533 0.064611 0.013441 ( 0.000041 0.000022 0.000027 ) -0.002363 -0.014557 0.066403 ( 0.000037 0.000020 0.000024 ) M - matrix: 0.004621 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004621 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004621 ( 0.000000 0.000000 0.000001 ) UB fit with 167 obs out of 178 (total:178,skipped:0) (93.82%) unit cell: 10.458(9) 10.426(4) 10.429(4) 89.94(3) 90.18(4) 89.87(5) V = 1137(1) unit cell: 10.4375(16) 10.4375(16) 10.4375(16) 90.0 90.0 90.0 V = 1137.1(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 167 obs out of 178 (total:178,skipped:0) (93.82%) 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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_51.rpb 0 of 164 peaks identified as outliers and rejected 164 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" 164 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8.tabbin file 164 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.93- 2.37 | 16 | 0.838 ( 0.098) | 0.814 ( 0.169) | 0.804 ( 0.396) | 2.14- 1.65 | 16 | 0.846 ( 0.104) | 0.843 ( 0.173) | 0.666 ( 0.160) | 1.65- 1.46 | 16 | 0.969 ( 0.105) | 1.015 ( 0.156) | 0.815 ( 0.371) | 1.36- 1.23 | 16 | 0.993 ( 0.076) | 1.049 ( 0.144) | 0.678 ( 0.242) | 1.23- 1.12 | 16 | 1.012 ( 0.091) | 0.995 ( 0.187) | 0.897 ( 0.378) | 1.11- 1.01 | 16 | 1.006 ( 0.097) | 1.068 ( 0.175) | 0.868 ( 0.349) | 1.00- 0.88 | 16 | 1.009 ( 0.075) | 1.049 ( 0.121) | 1.033 ( 0.372) | 0.88- 0.79 | 16 | 1.045 ( 0.075) | 1.061 ( 0.130) | 1.156 ( 0.477) | 0.79- 0.70 | 16 | 1.036 ( 0.060) | 1.061 ( 0.155) | 1.120 ( 0.399) | 0.70- 0.63 | 20 | 1.017 ( 0.057) | 0.926 ( 0.059) | 1.357 ( 0.556) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.93- 0.63 | 164 | 0.978 ( 0.110) | 0.987 ( 0.174) | 0.950 ( 0.447) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" UB fit with 164 obs out of 164 (total:164,skipped:0) (100.00%) UB - matrix: 0.065802 0.015601 0.005842 ( 0.000034 0.000019 0.000023 ) -0.016589 0.064506 0.013369 ( 0.000032 0.000018 0.000022 ) -0.002382 -0.014490 0.066502 ( 0.000022 0.000012 0.000015 ) M - matrix: 0.004611 -0.000009 0.000004 ( 0.000005 0.000003 0.000002 ) -0.000009 0.004614 -0.000010 ( 0.000003 0.000002 0.000002 ) 0.000004 -0.000010 0.004635 ( 0.000002 0.000002 0.000002 ) unit cell: 10.446(5) 10.442(3) 10.418(2) 89.87(2) 90.05(3) 89.89(3) V = 1136.3(7) OTKP changes: 164 1 1 1 OTKP changes: 164 1 1 1 OTKP changes: 164 1 1 1 No constraint UB - matrix: 0.065871 0.015584 0.005946 ( 0.000029 0.000016 0.000020 ) -0.016600 0.064667 0.013456 ( 0.000025 0.000014 0.000017 ) -0.002351 -0.014561 0.066484 ( 0.000020 0.000011 0.000013 ) M - matrix: 0.004620 -0.000013 0.000012 ( 0.000004 0.000002 0.000002 ) -0.000013 0.004637 -0.000005 ( 0.000002 0.000002 0.000001 ) 0.000012 -0.000005 0.004637 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.065871 0.015584 0.005946 ( 0.000029 0.000016 0.000020 ) -0.016600 0.064667 0.013456 ( 0.000025 0.000014 0.000017 ) -0.002351 -0.014561 0.066484 ( 0.000020 0.000011 0.000013 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000001 ) UB fit with 164 obs out of 164 (total:164,skipped:0) (100.00%) unit cell: 10.435(4) 10.417(2) 10.417(2) 89.936(18) 90.15(2) 89.84(2) V = 1132.3(6) unit cell: 10.4229(8) 10.4229(8) 10.4229(8) 90.0 90.0 90.0 V = 1132.31(14) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.156) HKL list info: 1010 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065871 0.015584 0.005946 ( 0.000029 0.000016 0.000020 ) -0.016600 0.064667 0.013456 ( 0.000025 0.000014 0.000017 ) -0.002351 -0.014561 0.066484 ( 0.000020 0.000011 0.000013 ) M - matrix: 0.004620 -0.000013 0.000012 ( 0.000004 0.000002 0.000002 ) -0.000013 0.004637 -0.000005 ( 0.000002 0.000002 0.000001 ) 0.000012 -0.000005 0.004637 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.065871 0.015584 0.005946 ( 0.000029 0.000016 0.000020 ) -0.016600 0.064667 0.013456 ( 0.000025 0.000014 0.000017 ) -0.002351 -0.014561 0.066484 ( 0.000020 0.000011 0.000013 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000001 ) UB fit with 164 obs out of 164 (total:164,skipped:0) (100.00%) unit cell: 10.435(4) 10.417(2) 10.417(2) 89.936(18) 90.15(2) 89.84(2) V = 1132.3(6) unit cell: 10.4229(8) 10.4229(8) 10.4229(8) 90.0 90.0 90.0 V = 1132.31(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 164 obs out of 164 (total:164,skipped:0) (100.00%) 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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_51.rpb 0 of 165 peaks identified as outliers and rejected 165 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" 165 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8.tabbin file 165 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.38 | 17 | 0.856 ( 0.097) | 0.849 ( 0.161) | 0.764 ( 0.447) | 2.38- 1.65 | 17 | 0.825 ( 0.111) | 0.813 ( 0.190) | 0.705 ( 0.158) | 1.65- 1.46 | 17 | 1.061 ( 0.399) | 1.138 ( 0.529) | 1.141 ( 1.656) | 1.36- 1.23 | 17 | 0.985 ( 0.076) | 1.029 ( 0.145) | 0.705 ( 0.225) | 1.20- 1.11 | 17 | 1.014 ( 0.094) | 1.023 ( 0.170) | 0.991 ( 0.448) | 1.11- 1.00 | 17 | 1.010 ( 0.090) | 1.037 ( 0.176) | 0.882 ( 0.374) | 1.00- 0.88 | 17 | 1.021 ( 0.078) | 1.072 ( 0.126) | 1.086 ( 0.422) | 0.88- 0.78 | 17 | 1.046 ( 0.071) | 1.063 ( 0.144) | 1.148 ( 0.461) | 0.75- 0.68 | 17 | 1.023 ( 0.060) | 0.994 ( 0.138) | 1.264 ( 0.475) | 0.68- 0.63 | 12 | 1.020 ( 0.065) | 0.937 ( 0.061) | 1.441 ( 0.560) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 165 | 0.985 ( 0.169) | 0.997 ( 0.243) | 1.000 ( 0.696) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.4 | 166 | 1.008 ( 0.132) | 1.063 ( 0.181) | 1.137 ( 0.696) | 10.6-15.2 | 166 | 1.001 ( 0.052) | 1.058 ( 0.074) | 1.079 ( 0.495) | 15.3-19.5 | 166 | 0.997 ( 0.168) | 1.040 ( 0.101) | 1.105 ( 0.898) | 19.5-23.7 | 166 | 0.977 ( 0.068) | 1.018 ( 0.090) | 0.929 ( 0.402) | 23.7-27.8 | 166 | 0.977 ( 0.070) | 1.018 ( 0.119) | 0.962 ( 0.444) | 27.9-32.7 | 166 | 0.953 ( 0.087) | 0.970 ( 0.122) | 0.938 ( 0.450) | 32.7-36.3 | 166 | 0.923 ( 0.151) | 0.916 ( 0.153) | 1.055 ( 0.631) | 36.4-38.9 | 166 | 0.892 ( 0.110) | 0.877 ( 0.234) | 1.016 ( 0.486) | 39.0-42.0 | 166 | 0.899 ( 0.112) | 0.850 ( 0.160) | 0.983 ( 0.447) | 42.0-50.2 | 168 | 0.873 ( 0.128) | 0.795 ( 0.148) | 0.943 ( 0.438) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.2 | 1662 | 0.950 ( 0.123) | 0.960 ( 0.171) | 1.015 ( 0.563) | Fitted profile normalization line parameters e1 dimension: a=-0.0033 b=1.14 e2 dimension: a=-0.0070 b=1.25 e3 dimension: a=0.0006 b=1.10 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_8" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 5011 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385971 Maximum peak integral for reflections I/sig<= 10000 - raw: 9693446 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 15:19:25 2019 PROFFITMAIN - Started at Wed Aug 21 15:19:25 2019 OTKP changes: 1296 2 7 8 OTKP changes: 1296 2 7 8 OTKP changes: 1296 2 7 8 No constraint UB - matrix: 0.066188 0.015223 0.006632 ( 0.000012 0.000012 0.000012 ) -0.016270 0.064845 0.013211 ( 0.000011 0.000011 0.000011 ) -0.003435 -0.014385 0.066490 ( 0.000014 0.000014 0.000015 ) M - matrix: 0.004657 0.000002 -0.000004 ( 0.000002 0.000001 0.000001 ) 0.000002 0.004643 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000004 0.000001 0.004639 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066188 0.015223 0.006632 ( 0.000012 0.000012 0.000012 ) -0.016270 0.064845 0.013211 ( 0.000011 0.000011 0.000011 ) -0.003435 -0.014385 0.066490 ( 0.000014 0.000014 0.000015 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000001 ) UB fit with 1368 obs out of 1662 (total:1662,skipped:0) (82.31%) unit cell: 10.3934(18) 10.4090(17) 10.414(2) 90.015(15) 89.946(16) 90.024(14) V = 1126.6(4) unit cell: 10.4053(6) 10.4053(6) 10.4053(6) 90.0 90.0 90.0 V = 1126.59(11) *** 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 187 obs out of 220 (total:220,skipped:0) (85.00%) UB - matrix: 0.066493 0.011697 0.008961 ( 0.000032 0.000042 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000030 0.000040 0.000034 ) -0.006060 -0.013937 0.065932 ( 0.000034 0.000046 0.000038 ) M - matrix: 0.004645 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000005 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.407(5) 10.500(6) 10.455(6) 90.60(5) 90.19(4) 89.65(4) V = 1142(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 No constraint UB - matrix: 0.066498 0.011700 0.008956 ( 0.000032 0.000042 0.000035 ) -0.013712 0.065062 0.013251 ( 0.000031 0.000042 0.000035 ) -0.006063 -0.013934 0.065958 ( 0.000034 0.000046 0.000038 ) M - matrix: 0.004647 -0.000030 0.000014 ( 0.000004 0.000004 0.000003 ) -0.000030 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000048 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011700 0.008956 ( 0.000032 0.000042 0.000035 ) -0.013712 0.065062 0.013251 ( 0.000031 0.000042 0.000035 ) -0.006063 -0.013934 0.065958 ( 0.000034 0.000046 0.000038 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000002 ) UB fit with 190 obs out of 220 (total:220,skipped:0) (86.36%) unit cell: 10.406(5) 10.500(6) 10.452(6) 90.60(5) 90.18(4) 89.63(4) V = 1142(1) unit cell: 10.4520(19) 10.4520(19) 10.4520(19) 90.0 90.0 90.0 V = 1141.8(3) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.127) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066498 0.011699 0.008956 ( 0.000032 0.000042 0.000035 ) -0.013712 0.065062 0.013251 ( 0.000031 0.000042 0.000035 ) -0.006063 -0.013934 0.065958 ( 0.000034 0.000046 0.000038 ) M - matrix: 0.004647 -0.000030 0.000014 ( 0.000004 0.000004 0.000003 ) -0.000030 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000048 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011699 0.008956 ( 0.000032 0.000042 0.000035 ) -0.013712 0.065062 0.013251 ( 0.000031 0.000042 0.000035 ) -0.006063 -0.013934 0.065958 ( 0.000034 0.000046 0.000038 ) M - matrix: 0.004628 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004628 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004628 ( 0.000000 0.000000 0.000002 ) UB fit with 190 obs out of 220 (total:220,skipped:0) (86.36%) unit cell: 10.406(5) 10.500(6) 10.452(6) 90.60(5) 90.18(4) 89.63(4) V = 1142(1) unit cell: 10.4520(19) 10.4520(19) 10.4520(19) 90.0 90.0 90.0 V = 1141.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 220 (total:220,skipped:0) (92.27%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068155 -0.000275 0.000125 ( 0.000028 0.000036 0.000029 ) -0.000050 0.067627 0.000627 ( 0.000031 0.000039 0.000032 ) -0.000030 -0.000056 0.067957 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004645 -0.000022 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000022 0.004574 0.000039 ( 0.000003 0.000005 0.000003 ) 0.000006 0.000039 0.004619 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068155 -0.000275 0.000125 ( 0.000028 0.000036 0.000029 ) -0.000050 0.067627 0.000627 ( 0.000031 0.000039 0.000032 ) -0.000030 -0.000056 0.067957 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 205 obs out of 220 (total:220,skipped:0) (93.18%) unit cell: 10.407(4) 10.489(6) 10.437(4) 90.48(4) 90.08(3) 89.72(4) V = 1139.3(9) unit cell: 10.4442(13) 10.4442(13) 10.4442(13) 90.0 90.0 90.0 V = 1139.3(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) UB - matrix: 0.066334 0.014185 0.006775 ( 0.000027 0.000035 0.000034 ) -0.015587 0.064701 0.012865 ( 0.000017 0.000023 0.000023 ) -0.004067 -0.014194 0.066894 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000010 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000010 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004686 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.471(3) 10.362(4) 89.74(3) 89.72(3) 89.88(3) V = 1127.3(7) OTKP changes: 255 1 1 1 OTKP changes: 255 1 1 1 No constraint UB - matrix: 0.066324 0.014177 0.006770 ( 0.000027 0.000035 0.000035 ) -0.015569 0.064673 0.012872 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014198 0.066868 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004658 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004585 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004683 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066324 0.014177 0.006770 ( 0.000027 0.000035 0.000035 ) -0.015569 0.064673 0.012872 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014198 0.066868 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) unit cell: 10.393(4) 10.475(3) 10.365(4) 89.74(3) 89.71(3) 89.89(3) V = 1128.4(7) unit cell: 10.4110(5) 10.4110(5) 10.4110(5) 90.0 90.0 90.0 V = 1128.44(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.030) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066324 0.014177 0.006770 ( 0.000027 0.000035 0.000035 ) -0.015569 0.064673 0.012872 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014198 0.066868 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004658 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004585 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004683 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066324 0.014177 0.006770 ( 0.000027 0.000035 0.000035 ) -0.015569 0.064673 0.012872 ( 0.000017 0.000023 0.000022 ) -0.004075 -0.014198 0.066868 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) unit cell: 10.393(4) 10.475(3) 10.365(4) 89.74(3) 89.71(3) 89.89(3) V = 1128.4(7) unit cell: 10.4110(5) 10.4110(5) 10.4110(5) 90.0 90.0 90.0 V = 1128.44(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068221 -0.000102 -0.000274 ( 0.000020 0.000026 0.000026 ) 0.000025 0.067866 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 0.000001 0.068348 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004654 -0.000005 -0.000019 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004606 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000019 -0.000011 0.004671 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068221 -0.000102 -0.000274 ( 0.000020 0.000026 0.000026 ) 0.000025 0.067866 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 0.000001 0.068348 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) UB fit with 255 obs out of 255 (total:255,skipped:0) (100.00%) unit cell: 10.397(3) 10.452(3) 10.378(3) 89.86(2) 89.76(2) 89.93(3) V = 1127.7(6) unit cell: 10.4088(5) 10.4088(5) 10.4088(5) 90.0 90.0 90.0 V = 1127.71(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065888 0.015209 0.006810 ( 0.000019 0.000013 0.000019 ) -0.016068 0.064791 0.013227 ( 0.000017 0.000012 0.000017 ) -0.003634 -0.014508 0.066503 ( 0.000021 0.000015 0.000021 ) M - matrix: 0.004613 0.000014 -0.000006 ( 0.000003 0.000001 0.000002 ) 0.000014 0.004640 -0.000004 ( 0.000001 0.000002 0.000002 ) -0.000006 -0.000004 0.004644 ( 0.000002 0.000002 0.000003 ) unit cell: 10.444(3) 10.413(2) 10.408(3) 89.948(19) 89.93(2) 90.170(19) V = 1132.0(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065938 0.015228 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016124 0.064850 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003637 -0.014463 0.066579 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004647 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065938 0.015228 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016124 0.064850 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003637 -0.014463 0.066579 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.434(3) 10.4056(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.8(5) unit cell: 10.4122(5) 10.4122(5) 10.4122(5) 90.0 90.0 90.0 V = 1128.81(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.029) HKL list info: 1275 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065938 0.015228 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016124 0.064850 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003637 -0.014463 0.066579 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004647 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065938 0.015228 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016124 0.064850 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003637 -0.014463 0.066579 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.434(3) 10.4056(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.8(5) unit cell: 10.4122(5) 10.4122(5) 10.4122(5) 90.0 90.0 90.0 V = 1128.81(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065938 0.015228 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016124 0.064850 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003637 -0.014463 0.066579 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004621 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004647 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004654 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065938 0.015228 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016124 0.064850 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003637 -0.014463 0.066579 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.434(3) 10.4056(19) 10.397(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.8(5) unit cell: 10.4122(5) 10.4122(5) 10.4122(5) 90.0 90.0 90.0 V = 1128.81(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 221 obs out of 221 (total:221,skipped:0) (100.00%) UB - matrix: 0.066122 0.015256 0.006584 ( 0.000015 0.000020 0.000017 ) -0.016340 0.064740 0.012923 ( 0.000012 0.000016 0.000013 ) -0.003349 -0.014204 0.066523 ( 0.000011 0.000014 0.000012 ) M - matrix: 0.004650 -0.000002 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000002 0.004626 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.004636 ( 0.000001 0.000001 0.000002 ) unit cell: 10.401(2) 10.429(2) 10.4178(19) 89.904(16) 90.017(17) 89.981(19) V = 1130.1(4) OTKP changes: 221 1 1 1 OTKP changes: 221 1 1 1 OTKP changes: 221 1 1 1 No constraint UB - matrix: 0.066157 0.015272 0.006524 ( 0.000013 0.000018 0.000015 ) -0.016369 0.064792 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003343 -0.014170 0.066615 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004656 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004632 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066157 0.015272 0.006524 ( 0.000013 0.000018 0.000015 ) -0.016369 0.064792 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003343 -0.014170 0.066615 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 221 obs out of 221 (total:221,skipped:0) (100.00%) unit cell: 10.395(2) 10.422(2) 10.4037(18) 89.945(16) 89.960(16) 89.965(18) V = 1127.1(4) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.029) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066157 0.015272 0.006524 ( 0.000013 0.000018 0.000015 ) -0.016369 0.064792 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003343 -0.014170 0.066615 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004656 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004632 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004648 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066157 0.015272 0.006524 ( 0.000013 0.000018 0.000015 ) -0.016369 0.064792 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003343 -0.014170 0.066615 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 221 obs out of 221 (total:221,skipped:0) (100.00%) unit cell: 10.395(2) 10.422(2) 10.4037(18) 89.945(16) 89.960(16) 89.965(18) V = 1127.1(4) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 221 (total:221,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068219 -0.000037 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000000 0.068074 -0.000053 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000009 0.068179 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004654 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004634 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068219 -0.000037 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000000 0.068074 -0.000053 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000009 0.068179 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 221 obs out of 221 (total:221,skipped:0) (100.00%) unit cell: 10.3974(16) 10.420(3) 10.4035(15) 89.963(16) 89.975(13) 89.969(17) V = 1127.1(4) unit cell: 10.4068(5) 10.4068(5) 10.4068(5) 90.0 90.0 90.0 V = 1127.07(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 265 obs out of 271 (total:271,skipped:0) (97.79%) UB - matrix: 0.065976 0.015330 0.006326 ( 0.000017 0.000012 0.000013 ) -0.016378 0.064795 0.013411 ( 0.000019 0.000015 0.000015 ) -0.002903 -0.014578 0.066490 ( 0.000019 0.000014 0.000015 ) M - matrix: 0.004629 -0.000008 0.000005 ( 0.000002 0.000002 0.000002 ) -0.000008 0.004646 -0.000003 ( 0.000002 0.000002 0.000001 ) 0.000005 -0.000003 0.004641 ( 0.000002 0.000001 0.000002 ) unit cell: 10.425(2) 10.406(2) 10.412(2) 89.959(18) 90.058(19) 89.907(19) V = 1129.5(4) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.066053 0.015389 0.006335 ( 0.000016 0.000012 0.000013 ) -0.016398 0.064851 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002878 -0.014635 0.066568 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004657 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004650 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066053 0.015389 0.006335 ( 0.000016 0.000012 0.000013 ) -0.016398 0.064851 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002878 -0.014635 0.066568 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.413(2) 10.394(2) 10.4014(18) 89.887(15) 90.093(17) 89.940(18) V = 1125.8(4) unit cell: 10.4028(5) 10.4028(5) 10.4028(5) 90.0 90.0 90.0 V = 1125.76(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.029) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066053 0.015389 0.006335 ( 0.000016 0.000012 0.000013 ) -0.016398 0.064851 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002878 -0.014635 0.066568 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004640 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004657 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004650 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066053 0.015389 0.006335 ( 0.000016 0.000012 0.000013 ) -0.016398 0.064851 0.013377 ( 0.000018 0.000013 0.000014 ) -0.002878 -0.014635 0.066568 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.413(2) 10.394(2) 10.4014(18) 89.887(15) 90.093(17) 89.940(18) V = 1125.8(4) unit cell: 10.4028(5) 10.4028(5) 10.4028(5) 90.0 90.0 90.0 V = 1125.76(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068124 -0.000095 0.000072 ( 0.000017 0.000013 0.000014 ) 0.000060 0.068209 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068186 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004641 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004652 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068124 -0.000095 0.000072 ( 0.000017 0.000013 0.000014 ) 0.000060 0.068209 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068186 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.412(3) 10.3989(16) 10.4025(18) 89.930(13) 90.044(17) 89.970(16) V = 1126.3(4) unit cell: 10.4044(5) 10.4044(5) 10.4044(5) 90.0 90.0 90.0 V = 1126.31(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 182 obs out of 190 (total:190,skipped:0) (95.79%) UB - matrix: 0.066064 0.015588 0.006256 ( 0.000020 0.000017 0.000019 ) -0.016422 0.064836 0.013095 ( 0.000027 0.000023 0.000026 ) -0.002976 -0.014215 0.066499 ( 0.000033 0.000028 0.000032 ) M - matrix: 0.004643 0.000007 0.000000 ( 0.000003 0.000002 0.000003 ) 0.000007 0.004649 0.000001 ( 0.000002 0.000003 0.000003 ) 0.000000 0.000001 0.004633 ( 0.000003 0.000003 0.000004 ) unit cell: 10.410(3) 10.403(4) 10.421(5) 90.02(3) 90.00(3) 90.09(3) V = 1128.5(7) OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 No constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004638 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.415(3) 10.421(3) 10.405(2) 89.85(2) 90.17(2) 90.10(2) V = 1129.2(5) unit cell: 10.4134(7) 10.4134(7) 10.4134(7) 90.0 90.0 90.0 V = 1129.23(13) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) HKL list info: 1267 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004638 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.415(3) 10.421(3) 10.405(2) 89.85(2) 90.17(2) 90.10(2) V = 1129.2(5) unit cell: 10.4134(7) 10.4134(7) 10.4134(7) 90.0 90.0 90.0 V = 1129.23(13) 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! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: 0.068131 0.000083 0.000194 ( 0.000020 0.000016 0.000019 ) -0.000013 0.068074 -0.000160 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068166 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000005 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000005 0.004634 -0.000011 ( 0.000002 0.000002 0.000002 ) 0.000013 -0.000011 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.068131 0.000083 0.000194 ( 0.000020 0.000016 0.000019 ) -0.000013 0.068074 -0.000160 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068166 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.411(3) 10.420(3) 10.4055(18) 89.867(19) 90.161(19) 90.06(2) V = 1128.7(5) unit cell: 10.4120(7) 10.4120(7) 10.4120(7) 90.0 90.0 90.0 V = 1128.75(12) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.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= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 88 obs out of 101 (total:101,skipped:0) (87.13%) UB - matrix: 0.066127 0.015352 0.006147 ( 0.000097 0.000048 0.000047 ) -0.016558 0.064626 0.013404 ( 0.000049 0.000025 0.000024 ) -0.002810 -0.014420 0.066466 ( 0.000082 0.000040 0.000040 ) M - matrix: 0.004655 -0.000014 -0.000002 ( 0.000013 0.000005 0.000006 ) -0.000014 0.004620 0.000002 ( 0.000005 0.000004 0.000003 ) -0.000002 0.000002 0.004635 ( 0.000006 0.000003 0.000005 ) unit cell: 10.396(14) 10.435(5) 10.418(6) 90.03(4) 89.97(8) 89.82(6) V = 1130(2) OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 No constraint UB - matrix: 0.066206 0.015411 0.005952 ( 0.000054 0.000029 0.000028 ) -0.016508 0.064724 0.013535 ( 0.000030 0.000016 0.000016 ) -0.002358 -0.014564 0.066553 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004661 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004639 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000001 0.004648 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066206 0.015411 0.005952 ( 0.000054 0.000029 0.000028 ) -0.016508 0.064724 0.013535 ( 0.000030 0.000016 0.000016 ) -0.002358 -0.014564 0.066553 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.389(8) 10.414(3) 10.404(3) 89.98(2) 90.17(3) 89.83(4) V = 1125.7(10) unit cell: 10.4024(9) 10.4024(9) 10.4024(9) 90.0 90.0 90.0 V = 1125.66(18) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.029) HKL list info: 674 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066206 0.015411 0.005952 ( 0.000054 0.000029 0.000028 ) -0.016508 0.064724 0.013535 ( 0.000030 0.000016 0.000016 ) -0.002358 -0.014564 0.066553 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004661 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004639 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000001 0.004648 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066206 0.015411 0.005952 ( 0.000054 0.000029 0.000028 ) -0.016508 0.064724 0.013535 ( 0.000030 0.000016 0.000016 ) -0.002358 -0.014564 0.066553 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.389(8) 10.414(3) 10.404(3) 89.98(2) 90.17(3) 89.83(4) V = 1125.7(10) unit cell: 10.4024(9) 10.4024(9) 10.4024(9) 90.0 90.0 90.0 V = 1125.66(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 7) ******* No constraint UB - matrix: 0.068280 -0.000192 0.000206 ( 0.000053 0.000028 0.000028 ) -0.000007 0.068108 -0.000019 ( 0.000031 0.000017 0.000016 ) 0.000000 -0.000002 0.068174 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004662 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004639 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000001 0.004648 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.068280 -0.000192 0.000206 ( 0.000053 0.000028 0.000028 ) -0.000007 0.068108 -0.000019 ( 0.000031 0.000017 0.000016 ) 0.000000 -0.000002 0.068174 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.388(8) 10.414(2) 10.404(3) 89.98(2) 90.17(4) 89.83(3) V = 1125.6(10) unit cell: 10.4022(9) 10.4022(9) 10.4022(9) 90.0 90.0 90.0 V = 1125.57(18) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 56.89 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb *** 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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_proffitpeak_8" UB fit with 154 obs out of 165 (total:165,skipped:0) (93.33%) UB - matrix: 0.065958 0.015565 0.005954 ( 0.000039 0.000022 0.000025 ) -0.016653 0.064709 0.013467 ( 0.000027 0.000015 0.000018 ) -0.002524 -0.014366 0.066547 ( 0.000045 0.000025 0.000030 ) M - matrix: 0.004634 -0.000015 0.000001 ( 0.000005 0.000002 0.000004 ) -0.000015 0.004636 0.000008 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000008 0.004645 ( 0.000004 0.000002 0.000004 ) unit cell: 10.420(6) 10.418(3) 10.407(4) 90.10(3) 90.01(4) 89.82(3) V = 1129.6(8) OTKP changes: 165 1 1 1 OTKP changes: 165 1 1 1 OTKP changes: 165 1 1 1 No constraint UB - matrix: 0.065995 0.015570 0.005941 ( 0.000031 0.000017 0.000021 ) -0.016572 0.064771 0.013500 ( 0.000025 0.000014 0.000017 ) -0.002335 -0.014598 0.066579 ( 0.000020 0.000011 0.000013 ) M - matrix: 0.004635 -0.000012 0.000013 ( 0.000004 0.000002 0.000002 ) -0.000012 0.004651 -0.000005 ( 0.000002 0.000002 0.000001 ) 0.000013 -0.000005 0.004650 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.065995 0.015570 0.005941 ( 0.000031 0.000017 0.000021 ) -0.016572 0.064771 0.013500 ( 0.000025 0.000014 0.000017 ) -0.002335 -0.014598 0.066579 ( 0.000020 0.000011 0.000013 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 165 obs out of 165 (total:165,skipped:0) (100.00%) unit cell: 10.418(4) 10.401(2) 10.401(2) 89.939(17) 90.16(2) 89.86(3) V = 1127.0(6) unit cell: 10.4067(7) 10.4067(7) 10.4067(7) 90.0 90.0 90.0 V = 1127.05(13) Run 8 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.029) HKL list info: 989 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065995 0.015570 0.005941 ( 0.000031 0.000017 0.000021 ) -0.016572 0.064771 0.013500 ( 0.000025 0.000014 0.000017 ) -0.002335 -0.014598 0.066579 ( 0.000020 0.000011 0.000013 ) M - matrix: 0.004635 -0.000012 0.000013 ( 0.000004 0.000002 0.000002 ) -0.000012 0.004651 -0.000005 ( 0.000002 0.000002 0.000001 ) 0.000013 -0.000005 0.004650 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.065995 0.015570 0.005941 ( 0.000031 0.000017 0.000021 ) -0.016572 0.064771 0.013500 ( 0.000025 0.000014 0.000017 ) -0.002335 -0.014598 0.066579 ( 0.000020 0.000011 0.000013 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 165 obs out of 165 (total:165,skipped:0) (100.00%) unit cell: 10.418(4) 10.401(2) 10.401(2) 89.939(17) 90.16(2) 89.86(3) V = 1127.0(6) unit cell: 10.4067(7) 10.4067(7) 10.4067(7) 90.0 90.0 90.0 V = 1127.05(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 165 obs out of 165 (total:165,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: 0.068072 -0.000156 0.000166 ( 0.000033 0.000018 0.000022 ) 0.000013 0.068191 -0.000055 ( 0.000020 0.000011 0.000013 ) -0.000020 0.000002 0.068184 ( 0.000020 0.000011 0.000014 ) M - matrix: 0.004634 -0.000010 0.000010 ( 0.000004 0.000002 0.000002 ) -0.000010 0.004650 -0.000004 ( 0.000002 0.000001 0.000001 ) 0.000010 -0.000004 0.004649 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.068072 -0.000156 0.000166 ( 0.000033 0.000018 0.000022 ) 0.000013 0.068191 -0.000055 ( 0.000020 0.000011 0.000013 ) -0.000020 0.000002 0.068184 ( 0.000020 0.000011 0.000014 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 165 obs out of 165 (total:165,skipped:0) (100.00%) unit cell: 10.420(5) 10.4016(16) 10.403(2) 89.956(14) 90.12(2) 89.88(2) V = 1127.5(6) unit cell: 10.4080(7) 10.4080(7) 10.4080(7) 90.0 90.0 90.0 V = 1127.48(13) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_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\xs2212a\tmp\xs2212a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_51.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068153 -0.000009 -0.000020 ( 0.000008 0.000008 0.000008 ) -0.000000 0.068104 0.000004 ( 0.000009 0.000008 0.000008 ) 0.000023 -0.000011 0.068176 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004645 -0.000001 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000001 0.004638 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000000 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068153 -0.000009 -0.000020 ( 0.000008 0.000008 0.000008 ) -0.000000 0.068104 0.000004 ( 0.000009 0.000008 0.000008 ) 0.000023 -0.000011 0.068176 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 1638 obs out of 1662 (total:1662,skipped:0) (98.56%) unit cell: 10.4074(13) 10.4150(12) 10.4039(9) 89.995(8) 90.002(9) 89.992(10) V = 1127.7(2) unit cell: 10.4088(3) 10.4088(3) 10.4088(3) 90.0 90.0 90.0 V = 1127.72(5) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 215 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_7.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_8.rrpprof 7315 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 15:19:43 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.127) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.030) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.029) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.029) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.029) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.029) Run 8 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.029) PROFFIT INFO: signal sum: min=-741.0000 max=7911371.0000 PROFFIT INFO: signal sum lp corr: min=-736.9381 max=1262890.6009 PROFFIT INFO: background sum: min=-104.0000 max=8336.0000 PROFFIT INFO: background sum sig2: min=423.0000 max=5810.0000 PROFFIT INFO: num of signal pixels: min=41 max=518 PROFFIT INFO: Inet: min=-1179.1011 max=2020625.0000 PROFFIT INFO: sig(Inet): min=52.0479 max=30724.9609 PROFFIT INFO: Inet/sig(Inet): min=-2.03 max=276.54 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 647 2493 3787 4535 4886 5686 6177 6470 6930 7238 7315 Percent 8.8 34.1 51.8 62.0 66.8 77.7 84.4 88.4 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 7315 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 7315 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2020625- 132713 731 414390.43 77.85 100.00 132194- 4066 731 29353.18 19.40 100.00 4065- 2132 731 2930.94 7.13 97.40 2131- 1258 731 1625.98 3.93 52.67 1257- 836 731 1029.20 2.37 16.42 835- 552 731 686.49 1.74 8.48 552- 345 731 447.23 1.24 4.65 345- 158 731 248.96 0.73 0.68 158- 18 731 83.06 0.30 0.00 17- -1179 736 -141.21 -0.27 0.00 ------------------------------------------------------------------------------------ 2020625- -1179 7315 45034.53 11.43 38.00 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 731 108676.36 15.49 67.44 1.64- 1.26 731 85921.67 20.95 57.32 1.26- 1.06 731 72819.49 21.27 71.00 1.06- 0.96 731 44220.62 12.37 30.51 0.96- 0.88 731 24883.17 8.99 46.65 0.88- 0.80 731 43346.70 12.26 34.20 0.80- 0.75 731 20394.65 6.20 20.52 0.75- 0.71 731 20994.64 6.82 16.55 0.71- 0.67 731 25557.87 8.20 29.41 0.67- 0.62 736 3812.04 1.85 6.66 ------------------------------------------------------------------------------------ 6.00- 0.62 7315 45034.53 11.43 38.00 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 15:19:43 2019 Sorting 7315 observations 55 unique observations with > 7.00 F2/sig(F2) 7315 observations in 8 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 8 0 74 736 Total number of frames 736 Maximum number of 55 frame scales suggested for reliable scaling Glued frame scales: 14 frame = 1 scale 7315 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 7 48 7 0 3 52 8 0 5 58 Total number of frames 58 1764 observations > 7.00 F2/sig(F2) 1764 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 6 47 7 0 3 51 8 0 5 57 Total number of frames 57 Removing 'redundancy=1' reflections Average redundancy: 24.1 (Out of 1764 removed 3 = 1761, unique = 73) 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 1761 observations in 8 runs Run # start # end # total # 1 0 7 8 2 0 7 16 3 0 7 24 4 0 7 32 5 0 7 40 6 0 6 47 7 0 3 51 8 0 5 57 Total number of frames 57 73 unique data precomputed (should be 73) 73 unique data with 1761 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 24.1 (Out of 1761 removed 0 = 1761, unique = 73) 73 unique data precomputed (should be 73) 73 unique data with 1761 observations RMS deviation of equivalent data = 0.30953 Rint = 0.25127 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24441, wR= 0.33397 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13629, wR= 0.18622, Acormin=0.479, Acormax=1.450, Acor_av=0.989 F test: Probability=1.000, F= 3.206 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13593, wR= 0.18218, Acormin=0.471, Acormax=1.495, Acor_av=0.981 F test: Probability=0.529, F= 1.004 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12641, wR= 0.17600, Acormin=0.547, Acormax=1.557, Acor_av=0.993 F test: Probability=0.998, F= 1.156 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12601, wR= 0.17082, Acormin=0.501, Acormax=1.569, Acor_av=0.986 F test: Probability=0.536, F= 1.004 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10558, wR= 0.15103, Acormin=0.566, Acormax=1.826, Acor_av=1.024 F test: Probability=1.000, F= 1.425 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11973, wR= 0.16894, Acormin=0.435, Acormax=1.651, Acor_av=0.976 F test: Probability=0.000, F= 0.776 Trying model 7 (ne=6, no=1)... Results: Rint= 0.11885, wR= 0.16476, Acormin=0.434, Acormax=1.631, Acor_av=0.972 F test: Probability=0.000, F= 0.786 Trying model 8 (ne=6, no=3)... Results: Rint= 0.10047, wR= 0.14746, Acormin=0.516, Acormax=1.825, Acor_av=1.008 F test: Probability=0.968, F= 1.096 Trying model 9 (ne=6, no=5)... Results: Rint= 0.15403, wR= 0.20038, Acormin=0.115, Acormax=1.229, Acor_av=0.530 F test: Probability=0.000, F= 0.423 Final absorption model (ne=6, no=3): Rint= 0.10047, Acormin=0.516, Acormax=1.825, Acor_av=1.008 Combined refinement in use Rint: 0.25317 There are 57 active scales (one needs to be fixed) Refinement control: frame scale #37 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 93 pars with 4371 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30953 Using Levenberg-Marquardt: 0.00010 New wR= 0.11109 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.25127 with corrections 0.08506 Rint for all data: 0.25317 with corrections 0.08775 6 observations identified as outliers and rejected Cycle 2 wR= 0.09825 Using Levenberg-Marquardt: 0.00001 New wR= 0.07675 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24947 with corrections 0.05751 Rint for all data: 0.25317 with corrections 0.06413 0 observations identified as outliers and rejected Cycle 3 wR= 0.07675 Using Levenberg-Marquardt: 0.00000 New wR= 0.07334 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24947 with corrections 0.05408 Rint for all data: 0.25317 with corrections 0.06027 0 observations identified as outliers and rejected Cycle 4 wR= 0.07334 Using Levenberg-Marquardt: 0.00000 New wR= 0.07177 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24947 with corrections 0.05300 Rint for all data: 0.25317 with corrections 0.05915 0 observations identified as outliers and rejected Cycle 5 wR= 0.07177 Using Levenberg-Marquardt: 0.00000 New wR= 0.07103 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24947 with corrections 0.05242 Rint for all data: 0.25317 with corrections 0.05848 0 observations identified as outliers and rejected Final wR= 0.07103 Final frame scales: Min= 0.6403 Max= 1.1808 Final absorption correction factors: Amin= 0.3275 Amax= 1.5850 PROFFIT INFO: Inet (after scale3 abspack): min=-1208.5385 max=1342404.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.8251 max=23554.1152 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/104 7315 reflections read from tmp file 265 reflections are rejected (264 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 1 4 4 2 4 5 2 216 Initial Chi^2= 0.53007 Cycle 1, Chi^2= 1.00273 Current error model SIG(F2)^2 = 57.29*I_RAW + 13.25*I_BACK+(0.04075*)^2 Cycle 2, Chi^2= 1.00966 Current error model SIG(F2)^2 = 72.32*I_RAW + 9.49*I_BACK+(0.03155*)^2 Cycle 3, Chi^2= 1.00753 Current error model SIG(F2)^2 = 80.50*I_RAW + 7.75*I_BACK+(0.02753*)^2 Cycle 4, Chi^2= 1.00423 Current error model SIG(F2)^2 = 84.57*I_RAW + 6.98*I_BACK+(0.02584*)^2 Cycle 5, Chi^2= 1.00191 Current error model SIG(F2)^2 = 86.35*I_RAW + 6.66*I_BACK+(0.02519*)^2 Cycle 6, Chi^2= 1.00076 Current error model SIG(F2)^2 = 87.06*I_RAW + 6.54*I_BACK+(0.02496*)^2 Cycle 7, Chi^2= 1.00028 Current error model SIG(F2)^2 = 87.33*I_RAW + 6.50*I_BACK+(0.02488*)^2 Cycle 8, Chi^2= 1.00010 Current error model SIG(F2)^2 = 87.42*I_RAW + 6.48*I_BACK+(0.02485*)^2 Final Chi^2= 1.00010 Final error model SIG(F2)^2 = 87.42*I_RAW + 6.48*I_BACK+(0.02485*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1342404- 119130 731 380987.71 31.71 100.00 118813- 3511 731 29356.31 13.06 100.00 3509- 2046 731 2717.95 6.14 98.91 2043- 1176 731 1526.35 3.93 66.62 1174- 780 731 960.28 2.77 26.95 780- 525 731 648.76 2.37 14.91 525- 329 731 422.91 1.96 8.89 329- 153 731 243.32 1.46 3.42 153- 16 731 81.14 0.73 0.27 16- -1209 736 -141.62 -0.56 0.00 ------------------------------------------------------------------------------------ 1342404- -1209 7315 41651.72 6.35 41.97 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 731 103289.07 10.30 71.14 1.64- 1.26 731 80351.21 9.39 60.19 1.26- 1.06 731 65940.91 9.35 75.51 1.06- 0.96 731 40998.15 5.88 32.83 0.96- 0.88 731 22513.57 5.68 53.49 0.88- 0.80 731 39969.29 6.78 40.90 0.80- 0.75 731 18357.41 4.10 23.26 0.75- 0.71 731 18903.84 4.82 20.79 0.71- 0.67 731 22897.19 5.51 32.97 0.67- 0.62 736 3557.16 1.74 8.83 ------------------------------------------------------------------------------------ 6.00- 0.62 7315 41651.72 6.35 41.97 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 731 103289.07 10.30 71.14 6.00- 1.26 1462 91820.14 9.84 65.66 6.00- 1.06 2193 83193.73 9.68 68.95 6.00- 0.96 2924 72644.84 8.73 59.92 6.00- 0.88 3655 62618.58 8.12 58.63 6.00- 0.80 4386 58843.70 7.89 55.68 6.00- 0.75 5117 53059.94 7.35 51.05 6.00- 0.71 5848 48790.43 7.04 47.26 6.00- 0.67 6579 45913.40 6.87 45.68 6.00- 0.62 7315 41651.72 6.35 41.97 ------------------------------------------------------------------------------------ 6.00- 0.62 7315 41651.72 6.35 41.97 Scale applied to data: s=0.744931 (maximum obs:1342404.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.058; Rsigma 0.037: data 7315 -> merged 241 With outlier rejection... Rint 0.051; Rsigma 0.037: data 7295 -> merged 241 Rejected total: 20, method kkm 10, method Blessing 10 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.622044, 6.009516 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.42 - 1.59 21 21 39.14 100.00 822 1.57 - 1.20 21 21 41.10 100.00 863 1.19 - 1.02 21 21 38.90 100.00 817 1.02 - 0.91 21 21 37.71 100.00 792 0.91 - 0.84 21 21 33.24 100.00 698 0.84 - 0.78 21 21 32.57 100.00 684 0.78 - 0.74 21 21 30.86 100.00 648 0.74 - 0.71 21 21 25.95 100.00 545 0.71 - 0.68 21 21 28.86 100.00 606 0.68 - 0.65 23 23 24.39 100.00 561 --------------------------------------------------------------- 10.42 - 0.65 212 212 33.19 100.00 7036 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 15:19:44 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.407437 10.415011 10.403915 89.9945 90.0025 89.9923 7295 Reflections read from file xs2212a.hkl 7295 Reflections used for space-group determination (up to diffraction limit of 0.62A); mean (I/sigma) = 6.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3657 0 4837 4832 7295 N (int>3sigma) = 0 0 0 0 1631 0 2145 2109 3055 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.6 29.9 30.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.4 6.3 6.3 Lattice type: F chosen Volume: 1127.72 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 0.5000 Unitcell: 7.358 7.358 7.360 119.98 119.97 90.02 Niggli form: a.a = 54.137 b.b = 54.141 c.c = 54.173 b.c = -27.063 a.c = -27.053 a.b = -0.018 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.085 CUBIC F-lattice R(int) = 0.051 [ 7054] Vol = 1127.7 Cell: 10.415 10.407 10.404 90.00 90.01 89.99 Volume: 1127.72 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.038 TETRAGONAL I-lattice R(int) = 0.051 [ 6656] Vol = 563.9 Cell: 7.361 7.362 10.404 90.00 89.99 89.96 Volume: 563.86 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.025 TETRAGONAL I-lattice R(int) = 0.051 [ 6653] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 89.99 90.02 Volume: 563.86 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.051 [ 6656] Vol = 563.9 Cell: 7.362 7.361 10.404 90.01 90.00 90.04 Volume: 563.86 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.011 ORTHORHOMBIC F-lattice R(int) = 0.050 [ 6602] Vol = 1127.7 Cell: 10.404 10.407 10.415 89.99 90.01 90.00 Volume: 1127.72 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.045 ORTHORHOMBIC I-lattice R(int) = 0.050 [ 6582] Vol = 563.9 Cell: 10.404 7.362 7.361 89.96 89.99 90.00 Volume: 563.86 Matrix: 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.025 ORTHORHOMBIC I-lattice R(int) = 0.050 [ 6582] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 90.01 90.02 Volume: 563.86 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) = 0.048 [ 6046] Vol = 563.9 Cell: 7.361 10.404 7.362 90.00 90.04 90.01 Volume: 563.86 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.010 MONOCLINIC I-lattice R(int) = 0.049 [ 6045] Vol = 563.9 Cell: 7.360 10.407 7.361 90.00 90.06 89.99 Volume: 563.86 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.006 MONOCLINIC I-lattice R(int) = 0.048 [ 6046] Vol = 563.9 Cell: 7.362 10.404 7.361 90.01 90.04 90.00 Volume: 563.86 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.020 MONOCLINIC I-lattice R(int) = 0.048 [ 6025] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 90.01 89.98 Volume: 563.86 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) = 0.048 [ 6043] Vol = 563.9 Cell: 7.358 10.415 7.358 90.00 90.02 89.99 Volume: 563.86 Matrix: 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.015 MONOCLINIC I-lattice R(int) = 0.048 [ 6043] Vol = 563.9 Cell: 7.358 10.415 7.358 90.00 90.02 90.01 Volume: 563.86 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) = 0.045 [ 4972] Vol = 281.9 Cell: 7.358 7.358 7.360 119.98 119.97 90.02 Volume: 281.93 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 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 3657 0 4837 4832 7295 N (int>3sigma) = 0 0 0 0 1631 0 2145 2109 3055 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.6 29.9 30.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.4 6.3 6.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.627 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 56 56 547 1429 N I>3s 2 2 2 762 0.0 0.0 0.0 1.9 0.8 0.8 0.2 4.9 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 0.051 6535 Fd-3m 1 1 227 C N N N N 37 2284 0.051 6601 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415011 10.407437 10.403915 89.9975 90.0055 89.9923 ZERR 5.00 0.001237 0.001293 0.000900 0.0086 0.0085 0.0099 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1130990- 127812 723 711 26 27.3 380714.05 31.73 0.047 0.062 109762- 3215 823 820 26 31.5 27557.27 12.35 0.064 0.076 3061- 1428 1055 1053 26 40.5 2263.19 5.57 0.128 0.182 1357- 865 926 926 26 35.6 1067.99 2.79 0.228 0.299 861- 527 879 879 26 33.8 653.72 2.32 0.315 0.430 521- 315 891 891 26 34.3 398.53 1.77 0.422 0.568 310- 139 677 675 26 26.0 235.83 1.33 0.564 0.924 134- 18 735 734 26 28.2 68.55 0.51 0.892 2.830 16- -217 606 606 33 18.4 -31.40 -0.08 0.994 5.292 ------------------------------------------------------------------------------------------- 1130990- -217 7315 7295 241 30.3 40819.32 6.30 0.051 0.067 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-1.44 1056 1051 26 40.4 114512.30 11.35 0.050 0.065 0.028 1.39-1.09 1119 1116 26 42.9 44160.39 7.46 0.043 0.057 0.033 1.06-0.94 936 933 26 35.9 39117.57 5.77 0.045 0.054 0.035 0.92-0.84 891 890 26 34.2 41252.53 7.53 0.050 0.067 0.040 0.84-0.78 865 864 26 33.2 24912.08 5.11 0.058 0.083 0.047 0.78-0.73 738 736 26 28.3 8998.56 3.19 0.080 0.101 0.074 0.73-0.69 738 737 26 28.3 19886.31 4.85 0.062 0.075 0.060 0.69-0.66 703 702 28 25.1 14099.62 3.76 0.075 0.100 0.068 0.65-0.62 269 266 31 8.6 8379.54 2.45 0.081 0.084 0.085 ------------------------------------------------------------------------------------------------------ inf-0.62 7315 7295 241 30.3 40819.32 6.30 0.051 0.067 0.037 inf-0.65 7051 7034 211 33.3 42084.91 6.46 0.051 0.066 0.037 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-1.44 1051 26 26 100.0 40.4 114512.30 72.21 0.050 0.005 1.39-1.09 1116 26 26 100.0 42.9 44160.39 44.30 0.043 0.006 1.06-0.94 933 26 26 100.0 35.9 39117.57 35.76 0.045 0.007 0.92-0.84 890 26 26 100.0 34.2 41252.53 43.41 0.050 0.008 0.84-0.78 864 26 26 100.0 33.2 24912.08 28.13 0.058 0.009 0.78-0.73 736 26 26 100.0 28.3 8998.56 17.20 0.080 0.015 0.73-0.69 737 26 26 100.0 28.3 19886.31 24.59 0.062 0.012 0.69-0.66 702 28 28 100.0 25.1 14099.62 20.29 0.075 0.014 0.65-0.62 266 32 31 96.9 8.6 8379.54 6.85 0.081 0.033 -------------------------------------------------------------------------------------------- inf-0.62 7295 242 241 99.6 30.3 40819.32 36.80 0.051 0.008 inf-0.65 7034 211 211 100.0 33.3 42084.91 37.94 0.051 0.007 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066103 0.015177 0.006658 ( 0.000008 0.000008 0.000008 ) -0.016239 0.064811 0.013211 ( 0.000009 0.000008 0.000008 ) -0.003386 -0.014395 0.066551 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004645 -0.000000 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000000 0.004638 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000001 0.004648 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066103 0.015177 0.006658 ( 0.000008 0.000008 0.000008 ) -0.016239 0.064811 0.013211 ( 0.000009 0.000008 0.000008 ) -0.003386 -0.014395 0.066551 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4076(13) 10.4150(12) 10.4040(9) 89.991(8) 90.003(9) 89.994(10) V = 1127.7(2) unit cell: 10.4089(3) 10.4089(3) 10.4089(3) 90.0 90.0 90.0 V = 1127.74(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.127) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.030) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.029) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.029) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.029) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.029) Run 8 Omega scan: (-49.000 - 26.000,75 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.029) PROFFIT INFO: signal sum: min=-741.0000 max=7911371.0000 PROFFIT INFO: signal sum lp corr: min=-736.9381 max=1262890.6009 PROFFIT INFO: background sum: min=-104.0000 max=8336.0000 PROFFIT INFO: background sum sig2: min=423.0000 max=5810.0000 PROFFIT INFO: num of signal pixels: min=41 max=518 PROFFIT INFO: Inet: min=-1179.1011 max=2020625.0000 PROFFIT INFO: sig(Inet): min=52.0479 max=30724.9609 PROFFIT INFO: Inet/sig(Inet): min=-2.03 max=276.54 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 1294 4986 7574 9070 9772 11372 12354 12940 13860 14476 14630 Percent 8.8 34.1 51.8 62.0 66.8 77.7 84.4 88.4 94.7 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 7315 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 7315 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2020625- 132713 731 414390.43 77.85 100.00 132194- 4066 731 29353.18 19.40 100.00 4065- 2132 731 2930.94 7.13 97.40 2131- 1258 731 1625.98 3.93 52.67 1257- 836 731 1029.20 2.37 16.42 835- 552 731 686.49 1.74 8.48 552- 345 731 447.23 1.24 4.65 345- 158 731 248.96 0.73 0.68 158- 18 731 83.06 0.30 0.00 17- -1179 736 -141.21 -0.27 0.00 ------------------------------------------------------------------------------------ 2020625- -1179 7315 45034.53 11.43 38.00 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 731 108676.36 15.49 67.44 1.64- 1.26 731 85921.67 20.95 57.32 1.26- 1.06 731 72819.49 21.27 71.00 1.06- 0.96 731 44220.62 12.37 30.51 0.96- 0.88 731 24883.17 8.99 46.65 0.88- 0.80 731 43346.70 12.26 34.20 0.80- 0.75 731 20394.65 6.20 20.52 0.75- 0.71 731 20994.64 6.82 16.55 0.71- 0.67 731 25557.87 8.20 29.41 0.67- 0.62 736 3812.04 1.85 6.66 ------------------------------------------------------------------------------------ 6.00- 0.62 7315 45034.53 11.43 38.00 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 15:19:44 2019 Sorting 7315 observations 44 unique observations with > 7.00 F2/sig(F2) 7315 observations in 8 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 8 0 74 736 Total number of frames 736 Maximum number of 44 frame scales suggested for reliable scaling Glued frame scales: 17 frame = 1 scale 7315 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 5 20 4 0 6 27 5 0 6 34 6 0 5 40 7 0 2 43 8 0 4 48 Total number of frames 48 1764 observations > 7.00 F2/sig(F2) 1764 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 5 13 3 0 5 19 4 0 6 26 5 0 6 33 6 0 5 39 7 0 2 42 8 0 4 47 Total number of frames 47 Removing 'redundancy=1' reflections Average redundancy: 30.9 (Out of 1764 removed 3 = 1761, unique = 57) 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 1761 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 5 13 3 0 5 19 4 0 6 26 5 0 6 33 6 0 5 39 7 0 2 42 8 0 4 47 Total number of frames 47 57 unique data precomputed (should be 57) 57 unique data with 1761 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 30.9 (Out of 1761 removed 0 = 1761, unique = 57) 57 unique data precomputed (should be 57) 57 unique data with 1761 observations RMS deviation of equivalent data = 0.30989 Rint = 0.25144 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.24458, wR= 0.33420 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13644, wR= 0.18686, Acormin=0.480, Acormax=1.451, Acor_av=0.989 F test: Probability=1.000, F= 3.204 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13598, wR= 0.18280, Acormin=0.471, Acormax=1.496, Acor_av=0.981 F test: Probability=0.542, F= 1.005 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12639, wR= 0.17696, Acormin=0.548, Acormax=1.556, Acor_av=0.994 F test: Probability=0.999, F= 1.159 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12602, wR= 0.17163, Acormin=0.504, Acormax=1.568, Acor_av=0.987 F test: Probability=0.533, F= 1.004 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10569, wR= 0.15182, Acormin=0.569, Acormax=1.827, Acor_av=1.024 F test: Probability=1.000, F= 1.422 Final absorption model (ne=4, no=3): Rint= 0.10569, Acormin=0.569, Acormax=1.827, Acor_av=1.024 Combined refinement in use Rint: 0.25335 There are 47 active scales (one needs to be fixed) Refinement control: frame scale #30 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 70 pars with 2485 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.30989 Using Levenberg-Marquardt: 0.00010 New wR= 0.11785 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.25144 with corrections 0.09073 Rint for all data: 0.25335 with corrections 0.09340 6 observations identified as outliers and rejected Cycle 2 wR= 0.10426 Using Levenberg-Marquardt: 0.00001 New wR= 0.08974 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.25145 with corrections 0.06728 Rint for all data: 0.25335 with corrections 0.07439 1 observations identified as outliers and rejected Cycle 3 wR= 0.08760 Using Levenberg-Marquardt: 0.00000 New wR= 0.08508 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.25097 with corrections 0.06253 Rint for all data: 0.25335 with corrections 0.06952 2 observations identified as outliers and rejected Cycle 4 wR= 0.07964 Using Levenberg-Marquardt: 0.00000 New wR= 0.07710 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24954 with corrections 0.05687 Rint for all data: 0.25335 with corrections 0.06435 1 observations identified as outliers and rejected Cycle 5 wR= 0.07310 Using Levenberg-Marquardt: 0.00000 New wR= 0.07035 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.24896 with corrections 0.05341 Rint for all data: 0.25335 with corrections 0.06087 0 observations identified as outliers and rejected Final wR= 0.07035 Final frame scales: Min= 0.8172 Max= 1.2627 Final absorption correction factors: Amin= 0.3345 Amax= 1.5502 PROFFIT INFO: Inet (after scale3 abspack): min=-1161.4811 max=1309848.2500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.6616 max=25909.0332 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/104 7315 reflections read from tmp file 308 reflections are rejected (307 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 1 1 1 2 2 5 0 150 Initial Chi^2= 0.51653 Cycle 1, Chi^2= 1.00303 Current error model SIG(F2)^2 = 59.43*I_RAW + 12.65*I_BACK+(0.03566*)^2 Cycle 2, Chi^2= 1.01071 Current error model SIG(F2)^2 = 72.53*I_RAW + 9.48*I_BACK+(0.02860*)^2 Cycle 3, Chi^2= 1.00429 Current error model SIG(F2)^2 = 76.94*I_RAW + 8.57*I_BACK+(0.02735*)^2 Cycle 4, Chi^2= 1.00109 Current error model SIG(F2)^2 = 78.08*I_RAW + 8.36*I_BACK+(0.02718*)^2 Cycle 5, Chi^2= 1.00025 Current error model SIG(F2)^2 = 78.34*I_RAW + 8.31*I_BACK+(0.02714*)^2 Cycle 6, Chi^2= 1.00006 Current error model SIG(F2)^2 = 78.40*I_RAW + 8.30*I_BACK+(0.02714*)^2 Final Chi^2= 1.00006 Final error model SIG(F2)^2 = 78.40*I_RAW + 8.30*I_BACK+(0.02714*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1309848- 118228 731 382303.25 30.46 100.00 117936- 3539 731 29311.40 13.38 100.00 3538- 2048 731 2740.25 6.43 99.45 2045- 1181 731 1535.90 4.08 72.09 1180- 787 731 966.38 2.88 31.19 785- 529 731 653.65 2.45 16.83 528- 332 731 425.84 1.98 8.76 331- 154 731 244.31 1.44 3.56 154- 17 731 81.51 0.70 0.27 17- -1161 736 -141.41 -0.56 0.00 ------------------------------------------------------------------------------------ 1309848- -1161 7315 41783.43 6.32 43.19 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 731 103603.12 10.18 71.41 1.64- 1.26 731 79665.15 9.27 60.88 1.26- 1.06 731 66506.48 9.22 76.33 1.06- 0.96 731 41245.22 5.74 33.79 0.96- 0.88 731 22803.25 5.72 56.22 0.88- 0.80 731 40257.53 6.72 42.68 0.80- 0.75 731 18393.62 4.11 24.21 0.75- 0.71 731 19135.26 4.86 22.85 0.71- 0.67 731 22940.67 5.62 34.06 0.67- 0.62 736 3545.56 1.78 9.65 ------------------------------------------------------------------------------------ 6.00- 0.62 7315 41783.43 6.32 43.19 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 731 103603.12 10.18 71.41 6.00- 1.26 1462 91634.13 9.73 66.14 6.00- 1.06 2193 83258.25 9.56 69.54 6.00- 0.96 2924 72754.99 8.61 60.60 6.00- 0.88 3655 62764.64 8.03 59.73 6.00- 0.80 4386 59013.46 7.81 56.89 6.00- 0.75 5117 53210.62 7.28 52.22 6.00- 0.71 5848 48951.20 6.98 48.55 6.00- 0.67 6579 46061.14 6.83 46.94 6.00- 0.62 7315 41783.43 6.32 43.19 ------------------------------------------------------------------------------------ 6.00- 0.62 7315 41783.43 6.32 43.19 Scale applied to data: s=0.763446 (maximum obs:1309848.250,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.061; Rsigma 0.038: data 7315 -> merged 163 With outlier rejection... Rint 0.056; Rsigma 0.038: data 7300 -> merged 163 Rejected total: 15, method kkm 7, method Blessing 8 Completeness direct cell (a, b, c) = (10.409, 10.409, 10.409), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.622048, 6.009559 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.42 - 1.76 14 14 47.14 100.00 660 1.73 - 1.27 14 14 51.57 100.00 722 1.26 - 1.06 14 14 59.21 100.00 829 1.05 - 0.97 14 14 51.29 100.00 718 0.95 - 0.88 14 14 54.14 100.00 758 0.87 - 0.81 14 14 48.14 100.00 674 0.80 - 0.76 14 14 50.50 100.00 707 0.76 - 0.72 14 14 41.79 100.00 585 0.72 - 0.69 14 14 46.50 100.00 651 0.69 - 0.65 19 19 38.74 100.00 736 --------------------------------------------------------------- 10.42 - 0.65 145 145 48.55 100.00 7040 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 15:19:44 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.407437 10.415011 10.403915 89.9945 90.0025 89.9923 7295 Reflections read from file xs2212a.hkl 7295 Reflections used for space-group determination (up to diffraction limit of 0.62A); mean (I/sigma) = 6.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3657 0 4837 4832 7295 N (int>3sigma) = 0 0 0 0 1631 0 2145 2109 3055 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.6 29.9 30.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.4 6.3 6.3 Lattice type: F chosen Volume: 1127.72 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 0.5000 Unitcell: 7.358 7.358 7.360 119.98 119.97 90.02 Niggli form: a.a = 54.137 b.b = 54.141 c.c = 54.173 b.c = -27.063 a.c = -27.053 a.b = -0.018 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.085 CUBIC F-lattice R(int) = 0.051 [ 7054] Vol = 1127.7 Cell: 10.415 10.407 10.404 90.00 90.01 89.99 Volume: 1127.72 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.038 TETRAGONAL I-lattice R(int) = 0.051 [ 6656] Vol = 563.9 Cell: 7.361 7.362 10.404 90.00 89.99 89.96 Volume: 563.86 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.025 TETRAGONAL I-lattice R(int) = 0.051 [ 6653] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 89.99 90.02 Volume: 563.86 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.051 [ 6656] Vol = 563.9 Cell: 7.362 7.361 10.404 90.01 90.00 90.04 Volume: 563.86 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.011 ORTHORHOMBIC F-lattice R(int) = 0.050 [ 6602] Vol = 1127.7 Cell: 10.404 10.407 10.415 89.99 90.01 90.00 Volume: 1127.72 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.045 ORTHORHOMBIC I-lattice R(int) = 0.050 [ 6582] Vol = 563.9 Cell: 10.404 7.362 7.361 89.96 89.99 90.00 Volume: 563.86 Matrix: 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.025 ORTHORHOMBIC I-lattice R(int) = 0.050 [ 6582] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 90.01 90.02 Volume: 563.86 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) = 0.048 [ 6046] Vol = 563.9 Cell: 7.361 10.404 7.362 90.00 90.04 90.01 Volume: 563.86 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.010 MONOCLINIC I-lattice R(int) = 0.049 [ 6045] Vol = 563.9 Cell: 7.360 10.407 7.361 90.00 90.06 89.99 Volume: 563.86 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.006 MONOCLINIC I-lattice R(int) = 0.048 [ 6046] Vol = 563.9 Cell: 7.362 10.404 7.361 90.01 90.04 90.00 Volume: 563.86 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.020 MONOCLINIC I-lattice R(int) = 0.048 [ 6025] Vol = 563.9 Cell: 7.358 7.358 10.415 90.00 90.01 89.98 Volume: 563.86 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) = 0.048 [ 6043] Vol = 563.9 Cell: 7.358 10.415 7.358 90.00 90.02 89.99 Volume: 563.86 Matrix: 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.015 MONOCLINIC I-lattice R(int) = 0.048 [ 6043] Vol = 563.9 Cell: 7.358 10.415 7.358 90.00 90.02 90.01 Volume: 563.86 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) = 0.045 [ 4972] Vol = 281.9 Cell: 7.358 7.358 7.360 119.98 119.97 90.02 Volume: 281.93 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 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 3657 0 4837 4832 7295 N (int>3sigma) = 0 0 0 0 1631 0 2145 2109 3055 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 31.6 29.9 30.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.0 0.0 6.4 6.3 6.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.627 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 56 56 547 1429 N I>3s 2 2 2 762 0.0 0.0 0.0 1.9 0.8 0.8 0.2 4.9 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 0.051 6535 Fd-3m 1 1 227 C N N N N 37 2284 0.051 6601 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.415011 10.407437 10.403915 89.9975 90.0055 89.9923 ZERR 5.00 0.001237 0.001293 0.000900 0.0086 0.0085 0.0099 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1142120- 95886 886 876 27 32.4 334244.25 28.83 0.053 0.068 79035- 1803 1374 1371 27 50.8 5317.40 8.60 0.087 0.093 1755- 777 1466 1465 27 54.3 1152.00 3.09 0.227 0.301 775- 333 1449 1448 27 53.6 509.16 2.09 0.360 0.505 332- 63 1127 1127 27 41.7 203.36 1.15 0.614 1.082 63- -192 1013 1013 28 36.2 1.17 0.10 0.979 5.132 ------------------------------------------------------------------------------------------- 1142120- -192 7315 7300 163 44.8 41471.70 6.30 0.056 0.071 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-1.27 1383 1380 27 51.1 95940.98 10.19 0.054 0.068 0.030 1.26-0.97 1552 1547 28 55.3 50268.12 7.07 0.049 0.064 0.035 0.95-0.81 1434 1432 28 51.1 32137.14 6.32 0.060 0.079 0.043 0.80-0.73 1265 1264 27 46.8 18589.64 4.44 0.062 0.077 0.054 0.72-0.67 1120 1118 27 41.4 18463.12 4.72 0.077 0.097 0.061 0.66-0.62 561 559 26 21.5 4330.28 1.88 0.103 0.077 0.118 ------------------------------------------------------------------------------------------------------ inf-0.62 7315 7300 163 44.8 41471.70 6.30 0.056 0.071 0.038 inf-0.65 7051 7038 144 48.9 42763.18 6.45 0.056 0.071 0.037 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-1.27 1380 27 27 100.0 51.1 95940.98 70.59 0.054 0.006 1.26-0.97 1547 28 28 100.0 55.3 50268.12 49.82 0.049 0.006 0.95-0.81 1432 28 28 100.0 51.1 32137.14 45.52 0.060 0.007 0.80-0.73 1264 27 27 100.0 46.8 18589.64 27.76 0.062 0.009 0.72-0.67 1118 27 27 100.0 41.4 18463.12 32.38 0.077 0.010 0.66-0.62 559 26 26 100.0 21.5 4330.28 8.80 0.103 0.026 -------------------------------------------------------------------------------------------- inf-0.62 7300 163 163 100.0 44.8 41471.70 43.27 0.056 0.007 inf-0.65 7038 144 144 100.0 48.9 42763.18 44.62 0.056 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Wed Aug 21 15:25:43 2019) ID: 3668; threads 39; handles 806; mem 511796.00 (1203668.00)kB; time: 1w 5d 1h 36m 31s MEMORY INFO: Memory PF:19.0, Ph:400.0, V:1175.0; MEMORY INFO: Process info - Handles: 807, Memory: PF:499.8,peak PF: 700.2, WS: 468.2, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:93.2 (#24) MEMORY INFO: Tracker: RED 94.4 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:20.0, Ph:400.0, V:1177.0; MEMORY INFO: Process info - Handles: 807, Memory: PF:501.6,peak PF: 700.2, WS: 470.0, peak WS: 637.0 MEMORY INFO: RED G:2.4,H:25.6 (#1114),V:95.0 (#25) MEMORY INFO: Tracker: RED 96.2 (#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 Wed Aug 21 15:25:43 2019 Experiment file name: D:\Data\xs2212a\xs2212a Output file name: D:\Data\xs2212a\xs2212a Data reduction with automatic settings UB - matrix: 0.066039 0.015016 0.006798 ( 0.000012 0.000012 0.000012 ) -0.015931 0.064696 0.013068 ( 0.000011 0.000011 0.000011 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000014 0.000014 ) 10.42433 ( 0.00178 ) 10.43788 ( 0.00170 ) 10.40727 ( 0.00214 ) 89.88512 ( 0.01498 ) 89.79539 ( 0.01523 ) 90.20497 ( 0.01354 ) V = 1132.38 Selected cell (from UM rr/UM ttt/UM f): 1 10.4243 10.4379 10.4073 89.8851 89.7954 90.2050 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\xs2212a\plots_red\xs2212a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs2212a\plots_red\xs2212a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs2212a\plots_red\xs2212a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs2212a\xs2212a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.16 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 Wed Aug 21 15:25:43 2019 Experiment file name: D:\Data\xs2212a\xs2212a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: 0.066039 0.015016 0.006798 ( 0.000012 0.000012 0.000012 ) -0.015931 0.064696 0.013068 ( 0.000011 0.000011 0.000011 ) -0.003867 -0.014380 0.066544 ( 0.000014 0.000014 0.000014 ) M - matrix: 0.004651 0.000001 -0.000003 ( 0.000002 0.000001 0.000001 ) 0.000001 0.004640 0.000000 ( 0.000001 0.000002 0.000001 ) -0.000003 0.000000 0.004642 ( 0.000001 0.000001 0.000002 ) unit cell: 10.4243(18) 10.4379(17) 10.407(2) 89.885(15) 89.795(15) 90.205(14) V = 1132.4(3) unit cell: 10.4083(5) 10.4083(5) 10.4083(5) 90.0 90.0 90.0 V = 1127.56(10) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" UB fit with 53 obs out of 232 (total:232,skipped:0) (22.84%) UB - matrix: 0.065934 0.014901 0.006882 ( 0.000121 0.000099 0.000125 ) -0.015866 0.064673 0.013139 ( 0.000175 0.000143 0.000181 ) -0.003967 -0.014334 0.066197 ( 0.000209 0.000171 0.000217 ) M - matrix: 0.004615 0.000013 -0.000017 ( 0.000017 0.000014 0.000017 ) 0.000013 0.004610 0.000003 ( 0.000014 0.000019 0.000017 ) -0.000017 0.000003 0.004602 ( 0.000017 0.000017 0.000029 ) unit cell: 10.441(19) 10.45(2) 10.46(3) 90.0(2) 89.8(2) 90.17(17) V = 1140(5) ********************** SEARCHING FOR BEST UB STARTED ********************* UM IRUN INFO: Rotation interval: [-2.00,2.00] (deg), number of steps 17, indexing rejection criterion: 0.1250 UM IRUN INFO: There are 1 'run' pieces in the peak table RUN 1, #refl in peak table: 232 #indexed refl 162, indexation with best UB: 69.8276% Lattice: 10.4135 10.4640 10.4681 90.456 89.847 89.845 1140.630 Rotation: 12.175 -5.371 11.360 ********************** SEARCHING FOR BEST UB ENDED *********************** UB fit with 160 obs out of 232 (total:232,skipped:0) (68.97%) UB - matrix: 0.066514 0.011437 0.008923 ( 0.000044 0.000057 0.000048 ) -0.013367 0.065285 0.013322 ( 0.000038 0.000049 0.000041 ) -0.006346 -0.014176 0.065827 ( 0.000042 0.000055 0.000046 ) M - matrix: 0.004643 -0.000022 -0.000002 ( 0.000006 0.000005 0.000004 ) -0.000022 0.004594 0.000039 ( 0.000005 0.000007 0.000005 ) -0.000002 0.000039 0.004590 ( 0.000004 0.000005 0.000006 ) unit cell: 10.410(7) 10.466(7) 10.470(7) 90.48(6) 89.97(5) 89.73(6) V = 1141(1) OTKP changes: 76 1 1 1 OTKP changes: 76 1 1 1 UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013470 0.064976 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006250 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) UB - matrix: 0.066169 0.011500 0.009068 ( 0.000042 0.000055 0.000046 ) -0.013469 0.064977 0.013267 ( 0.000035 0.000045 0.000038 ) -0.006251 -0.014113 0.065726 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004599 -0.000026 0.000010 ( 0.000006 0.000004 0.000004 ) -0.000026 0.004553 0.000039 ( 0.000004 0.000006 0.000004 ) 0.000010 0.000039 0.004578 ( 0.000004 0.000004 0.000006 ) unit cell: 10.460(7) 10.512(7) 10.483(7) 90.49(5) 90.13(5) 89.67(5) V = 1153(1) OTKP changes: 79 1 1 1 OTKP changes: 79 1 1 1 UB - matrix: 0.066060 0.011531 0.009083 ( 0.000042 0.000055 0.000047 ) -0.013516 0.064862 0.013265 ( 0.000033 0.000043 0.000036 ) -0.006188 -0.014092 0.065671 ( 0.000040 0.000052 0.000044 ) M - matrix: 0.004585 -0.000028 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000028 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.475(7) 10.529(7) 10.492(7) 90.50(5) 90.18(5) 89.65(5) V = 1157(1) Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.441) HKL list info: 1331 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066056 0.011526 0.009080 ( 0.000042 0.000055 0.000047 ) -0.013495 0.064867 0.013272 ( 0.000034 0.000044 0.000038 ) -0.006199 -0.014097 0.065666 ( 0.000040 0.000053 0.000045 ) M - matrix: 0.004584 -0.000027 0.000014 ( 0.000006 0.000004 0.000004 ) -0.000027 0.004539 0.000040 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000040 0.004571 ( 0.000004 0.000004 0.000006 ) UB fit with 164 obs out of 232 (total:232,skipped:0) (70.69%) unit cell: 10.477(7) 10.528(7) 10.492(7) 90.50(5) 90.17(5) 89.66(5) V = 1157(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 176 obs out of 232 (total:232,skipped:0) (75.86%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 213 peaks identified as outliers and rejected 213 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 213 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 213 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 2.99 | 21 | 0.974 ( 0.495) | 0.839 ( 0.189) | 1.386 ( 1.508) | 2.64- 1.77 | 21 | 0.825 ( 0.087) | 0.820 ( 0.149) | 0.786 ( 0.427) | 1.77- 1.59 | 21 | 0.879 ( 0.124) | 0.887 ( 0.146) | 0.652 ( 0.260) | 1.59- 1.37 | 21 | 0.923 ( 0.076) | 0.998 ( 0.128) | 1.154 ( 0.688) | 1.37- 1.20 | 21 | 0.918 ( 0.078) | 0.972 ( 0.128) | 1.021 ( 0.709) | 1.17- 1.01 | 21 | 0.935 ( 0.094) | 0.962 ( 0.172) | 0.824 ( 0.212) | 1.01- 0.89 | 21 | 0.957 ( 0.075) | 1.001 ( 0.117) | 1.192 ( 0.474) | 0.89- 0.83 | 21 | 0.979 ( 0.074) | 1.040 ( 0.147) | 1.221 ( 0.472) | 0.83- 0.72 | 21 | 0.967 ( 0.038) | 0.960 ( 0.112) | 1.220 ( 0.421) | 0.72- 0.64 | 24 | 0.956 ( 0.044) | 0.918 ( 0.073) | 1.303 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.07- 0.64 | 213 | 0.932 ( 0.179) | 0.939 ( 0.155) | 1.079 ( 0.702) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 176 obs out of 213 (total:213,skipped:0) (82.63%) UB - matrix: 0.066165 0.011574 0.009057 ( 0.000036 0.000046 0.000035 ) -0.013599 0.064713 0.013260 ( 0.000033 0.000043 0.000033 ) -0.006039 -0.014149 0.065558 ( 0.000039 0.000050 0.000038 ) M - matrix: 0.004599 -0.000029 0.000023 ( 0.000005 0.000004 0.000004 ) -0.000029 0.004522 0.000035 ( 0.000004 0.000006 0.000004 ) 0.000023 0.000035 0.004556 ( 0.000004 0.000004 0.000005 ) unit cell: 10.459(6) 10.548(7) 10.509(6) 90.45(5) 90.29(4) 89.64(5) V = 1159(1) OTKP changes: 184 1 1 1 OTKP changes: 184 1 1 1 No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1323 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004645 -0.000026 0.000014 ( 0.000005 0.000004 0.000003 ) -0.000026 0.004569 0.000044 ( 0.000004 0.000006 0.000004 ) 0.000014 0.000044 0.004606 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066490 0.011706 0.008967 ( 0.000033 0.000044 0.000035 ) -0.013669 0.065091 0.013224 ( 0.000032 0.000042 0.000033 ) -0.006084 -0.013968 0.065958 ( 0.000035 0.000046 0.000036 ) M - matrix: 0.004627 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004627 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004627 ( 0.000000 0.000000 0.000001 ) UB fit with 186 obs out of 213 (total:213,skipped:0) (87.32%) unit cell: 10.408(5) 10.494(6) 10.452(6) 90.56(5) 90.18(4) 89.67(4) V = 1142(1) unit cell: 10.4510(16) 10.4510(16) 10.4510(16) 90.0 90.0 90.0 V = 1141.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 196 obs out of 213 (total:213,skipped:0) (92.02%) 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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.rpb 0 of 220 peaks identified as outliers and rejected 220 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" 220 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1.tabbin file 220 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.61 | 22 | 0.994 ( 0.545) | 0.875 ( 0.217) | 1.604 ( 2.396) | 2.60- 1.76 | 22 | 0.826 ( 0.089) | 0.812 ( 0.146) | 0.797 ( 0.423) | 1.76- 1.57 | 22 | 0.859 ( 0.092) | 0.892 ( 0.147) | 0.750 ( 0.322) | 1.57- 1.35 | 22 | 0.916 ( 0.076) | 0.975 ( 0.139) | 1.025 ( 0.503) | 1.35- 1.16 | 22 | 0.955 ( 0.072) | 1.030 ( 0.124) | 1.029 ( 0.678) | 1.16- 1.01 | 22 | 0.911 ( 0.085) | 0.938 ( 0.170) | 0.923 ( 0.398) | 1.01- 0.88 | 22 | 0.957 ( 0.073) | 1.004 ( 0.124) | 1.180 ( 0.493) | 0.88- 0.79 | 22 | 0.985 ( 0.059) | 1.028 ( 0.140) | 1.234 ( 0.387) | 0.79- 0.70 | 22 | 0.984 ( 0.041) | 0.962 ( 0.107) | 1.276 ( 0.475) | 0.70- 0.63 | 22 | 0.943 ( 0.038) | 0.917 ( 0.081) | 1.311 ( 0.481) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 220 | 0.933 ( 0.193) | 0.943 ( 0.158) | 1.113 ( 0.914) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) UB fit with 218 obs out of 277 (total:277,skipped:0) (78.70%) UB - matrix: 0.066106 0.014703 0.007006 ( 0.000030 0.000045 0.000053 ) -0.015623 0.064647 0.012967 ( 0.000027 0.000041 0.000047 ) -0.004077 -0.014389 0.066675 ( 0.000029 0.000044 0.000051 ) M - matrix: 0.004631 0.000021 -0.000011 ( 0.000004 0.000004 0.000004 ) 0.000021 0.004602 -0.000018 ( 0.000004 0.000006 0.000004 ) -0.000011 -0.000018 0.004663 ( 0.000004 0.000004 0.000007 ) unit cell: 10.424(5) 10.456(6) 10.388(8) 89.78(5) 89.86(5) 90.26(4) V = 1132(1) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 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 fit with 246 obs out of 277 (total:277,skipped:0) (88.81%) UB - matrix: 0.066185 0.014322 0.006899 ( 0.000029 0.000040 0.000044 ) -0.015499 0.064550 0.012796 ( 0.000026 0.000036 0.000040 ) -0.004103 -0.014251 0.066778 ( 0.000027 0.000037 0.000040 ) M - matrix: 0.004638 0.000006 -0.000016 ( 0.000004 0.000003 0.000003 ) 0.000006 0.004575 -0.000027 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000027 0.004671 ( 0.000003 0.000004 0.000006 ) unit cell: 10.416(5) 10.487(6) 10.379(6) 89.67(4) 89.81(4) 90.07(4) V = 1134(1) OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 OTKP changes: 95 1 1 1 UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066144 0.014185 0.006828 ( 0.000029 0.000039 0.000043 ) -0.015501 0.064537 0.012733 ( 0.000028 0.000038 0.000041 ) -0.004051 -0.014233 0.066756 ( 0.000026 0.000035 0.000038 ) M - matrix: 0.004632 -0.000004 -0.000016 ( 0.000004 0.000003 0.000003 ) -0.000004 0.004569 -0.000032 ( 0.000003 0.000005 0.000004 ) -0.000016 -0.000032 0.004665 ( 0.000003 0.000004 0.000005 ) UB fit with 252 obs out of 277 (total:277,skipped:0) (90.97%) unit cell: 10.422(5) 10.494(6) 10.385(6) 89.61(4) 89.80(4) 89.94(4) V = 1136(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 253 obs out of 277 (total:277,skipped:0) (91.34%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 252 peaks identified as outliers and rejected 252 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 252 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 252 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 2.37 | 25 | 0.863 ( 0.090) | 0.867 ( 0.127) | 1.007 ( 0.459) | 2.37- 1.76 | 25 | 0.879 ( 0.100) | 0.894 ( 0.146) | 0.990 ( 0.542) | 1.76- 1.58 | 25 | 0.897 ( 0.093) | 0.877 ( 0.150) | 0.946 ( 0.406) | 1.58- 1.35 | 25 | 0.934 ( 0.081) | 0.964 ( 0.111) | 0.839 ( 0.341) | 1.35- 1.19 | 25 | 0.917 ( 0.073) | 0.918 ( 0.101) | 0.936 ( 0.530) | 1.19- 1.09 | 25 | 0.935 ( 0.061) | 0.960 ( 0.113) | 0.869 ( 0.325) | 1.09- 0.92 | 25 | 0.954 ( 0.071) | 0.975 ( 0.101) | 1.053 ( 0.460) | 0.91- 0.82 | 25 | 0.936 ( 0.069) | 0.935 ( 0.090) | 1.089 ( 0.386) | 0.82- 0.73 | 25 | 0.949 ( 0.053) | 0.894 ( 0.084) | 1.434 ( 0.441) | 0.72- 0.63 | 27 | 0.930 ( 0.034) | 0.885 ( 0.092) | 1.347 ( 0.476) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.99- 0.63 | 252 | 0.919 ( 0.080) | 0.917 ( 0.119) | 1.053 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) UB - matrix: 0.066197 0.014136 0.006718 ( 0.000026 0.000033 0.000033 ) -0.015599 0.064670 0.012816 ( 0.000017 0.000022 0.000022 ) -0.003913 -0.014173 0.066842 ( 0.000023 0.000030 0.000029 ) M - matrix: 0.004641 -0.000018 -0.000017 ( 0.000003 0.000003 0.000003 ) -0.000018 0.004583 -0.000024 ( 0.000003 0.000003 0.000003 ) -0.000017 -0.000024 0.004677 ( 0.000003 0.000003 0.000004 ) unit cell: 10.412(4) 10.478(3) 10.372(4) 89.71(3) 89.79(3) 89.78(3) V = 1131.5(7) OTKP changes: 252 1 1 1 OTKP changes: 252 1 1 1 No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.006) HKL list info: 1311 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004659 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004588 -0.000022 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000022 0.004686 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066333 0.014187 0.006776 ( 0.000027 0.000035 0.000034 ) -0.015578 0.064691 0.012855 ( 0.000017 0.000022 0.000022 ) -0.004079 -0.014203 0.066894 ( 0.000018 0.000024 0.000023 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) unit cell: 10.391(4) 10.472(3) 10.362(4) 89.72(3) 89.71(3) 89.89(3) V = 1127.5(7) unit cell: 10.4082(5) 10.4082(5) 10.4082(5) 90.0 90.0 90.0 V = 1127.53(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 252 obs out of 252 (total:252,skipped:0) (100.00%) 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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.rpb 0 of 254 peaks identified as outliers and rejected 254 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" 254 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2.tabbin file 254 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 2.38 | 25 | 0.868 ( 0.089) | 0.871 ( 0.125) | 1.025 ( 0.501) | 2.37- 1.75 | 25 | 0.880 ( 0.098) | 0.899 ( 0.143) | 1.013 ( 0.546) | 1.75- 1.58 | 25 | 0.891 ( 0.092) | 0.870 ( 0.151) | 0.984 ( 0.404) | 1.58- 1.35 | 25 | 0.943 ( 0.085) | 0.965 ( 0.115) | 0.908 ( 0.435) | 1.35- 1.19 | 25 | 0.914 ( 0.070) | 0.918 ( 0.101) | 0.977 ( 0.540) | 1.19- 1.09 | 25 | 0.943 ( 0.062) | 0.974 ( 0.116) | 0.888 ( 0.377) | 1.09- 0.92 | 25 | 0.949 ( 0.080) | 0.981 ( 0.099) | 1.019 ( 0.446) | 0.92- 0.87 | 25 | 0.945 ( 0.067) | 0.936 ( 0.094) | 1.074 ( 0.403) | 0.86- 0.73 | 25 | 0.958 ( 0.050) | 0.919 ( 0.091) | 1.335 ( 0.450) | 0.73- 0.63 | 29 | 0.929 ( 0.037) | 0.880 ( 0.095) | 1.340 ( 0.463) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.00- 0.63 | 254 | 0.922 ( 0.081) | 0.921 ( 0.121) | 1.061 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) UB fit with 230 obs out of 253 (total:253,skipped:0) (90.91%) UB - matrix: 0.065895 0.015172 0.006767 ( 0.000035 0.000024 0.000033 ) -0.016081 0.064693 0.013183 ( 0.000026 0.000018 0.000025 ) -0.003711 -0.014447 0.066447 ( 0.000033 0.000022 0.000031 ) M - matrix: 0.004615 0.000013 -0.000013 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000013 -0.000004 0.004635 ( 0.000003 0.000002 0.000004 ) unit cell: 10.442(5) 10.431(3) 10.419(5) 89.95(3) 89.84(4) 90.16(3) V = 1134.8(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) UB - matrix: 0.065880 0.015187 0.006743 ( 0.000036 0.000025 0.000035 ) -0.016086 0.064688 0.013200 ( 0.000025 0.000017 0.000024 ) -0.003694 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004613 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.83(4) 90.17(3) V = 1134.9(8) OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 OTKP changes: 93 1 1 1 Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1295 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065878 0.015187 0.006735 ( 0.000036 0.000025 0.000034 ) -0.016086 0.064688 0.013207 ( 0.000025 0.000017 0.000023 ) -0.003693 -0.014455 0.066453 ( 0.000032 0.000022 0.000031 ) M - matrix: 0.004612 0.000013 -0.000014 ( 0.000005 0.000002 0.000003 ) 0.000013 0.004624 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000014 -0.000004 0.004636 ( 0.000003 0.000002 0.000004 ) UB fit with 233 obs out of 253 (total:253,skipped:0) (92.09%) unit cell: 10.444(5) 10.431(3) 10.418(5) 89.95(3) 89.82(4) 90.16(3) V = 1134.9(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 232 obs out of 253 (total:253,skipped:0) (91.70%) 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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 240 peaks identified as outliers and rejected 240 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 240 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 240 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 2.37 | 24 | 0.865 ( 0.095) | 0.881 ( 0.138) | 1.198 ( 0.640) | 2.36- 1.76 | 24 | 0.899 ( 0.097) | 0.918 ( 0.146) | 0.989 ( 0.481) | 1.76- 1.58 | 24 | 0.923 ( 0.081) | 0.960 ( 0.120) | 0.783 ( 0.283) | 1.58- 1.35 | 24 | 0.940 ( 0.072) | 0.952 ( 0.134) | 0.953 ( 0.521) | 1.35- 1.19 | 24 | 0.969 ( 0.064) | 1.004 ( 0.109) | 0.941 ( 0.487) | 1.16- 1.04 | 24 | 0.967 ( 0.065) | 0.990 ( 0.118) | 0.952 ( 0.447) | 1.01- 0.88 | 24 | 0.964 ( 0.084) | 0.994 ( 0.101) | 0.994 ( 0.402) | 0.88- 0.82 | 24 | 0.996 ( 0.058) | 0.999 ( 0.125) | 0.900 ( 0.360) | 0.79- 0.69 | 24 | 0.995 ( 0.045) | 0.998 ( 0.128) | 1.290 ( 0.494) | 0.69- 0.63 | 24 | 0.976 ( 0.051) | 0.910 ( 0.100) | 1.242 ( 0.513) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.87- 0.63 | 240 | 0.949 ( 0.084) | 0.961 ( 0.130) | 1.024 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) UB - matrix: 0.065959 0.015264 0.006743 ( 0.000021 0.000015 0.000020 ) -0.016095 0.064720 0.013251 ( 0.000015 0.000011 0.000015 ) -0.003618 -0.014638 0.066528 ( 0.000028 0.000019 0.000027 ) M - matrix: 0.004623 0.000018 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000018 0.004636 -0.000013 ( 0.000001 0.000002 0.000002 ) -0.000009 -0.000013 0.004647 ( 0.000002 0.000002 0.000004 ) unit cell: 10.432(3) 10.4176(19) 10.405(4) 89.84(2) 89.89(3) 90.223(19) V = 1130.8(6) OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 OTKP changes: 240 1 1 1 No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.156) HKL list info: 1294 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004606 0.000011 -0.000010 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004630 0.000001 ( 0.000001 0.000002 0.000001 ) -0.000010 0.000001 0.004638 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065833 0.015164 0.006791 ( 0.000019 0.000013 0.000018 ) -0.016064 0.064740 0.013258 ( 0.000016 0.000011 0.000016 ) -0.003675 -0.014458 0.066455 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 240 obs out of 240 (total:240,skipped:0) (100.00%) unit cell: 10.452(3) 10.4239(19) 10.415(3) 90.007(18) 89.87(2) 90.142(18) V = 1134.7(5) unit cell: 10.4302(6) 10.4302(6) 10.4302(6) 90.0 90.0 90.0 V = 1134.68(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 240 obs out of 240 (total:240,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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.rpb 0 of 239 peaks identified as outliers and rejected 239 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" 239 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3.tabbin file 239 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.38 | 24 | 0.878 ( 0.087) | 0.900 ( 0.122) | 1.206 ( 0.670) | 2.38- 1.76 | 24 | 0.890 ( 0.105) | 0.905 ( 0.160) | 0.976 ( 0.480) | 1.76- 1.59 | 24 | 0.901 ( 0.093) | 0.931 ( 0.143) | 0.766 ( 0.307) | 1.59- 1.36 | 24 | 0.959 ( 0.067) | 1.002 ( 0.107) | 0.998 ( 0.531) | 1.36- 1.19 | 24 | 0.950 ( 0.071) | 0.964 ( 0.140) | 0.922 ( 0.493) | 1.19- 1.05 | 24 | 0.973 ( 0.058) | 0.996 ( 0.109) | 0.962 ( 0.437) | 1.05- 0.88 | 24 | 0.973 ( 0.059) | 1.015 ( 0.108) | 1.054 ( 0.488) | 0.88- 0.79 | 24 | 1.000 ( 0.050) | 0.992 ( 0.112) | 0.915 ( 0.347) | 0.79- 0.70 | 24 | 0.997 ( 0.045) | 1.003 ( 0.139) | 1.318 ( 0.486) | 0.70- 0.63 | 23 | 0.976 ( 0.053) | 0.916 ( 0.110) | 1.237 ( 0.520) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 239 | 0.950 ( 0.083) | 0.963 ( 0.133) | 1.034 ( 0.511) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) UB fit with 200 obs out of 238 (total:238,skipped:0) (84.03%) UB - matrix: 0.066082 0.015217 0.006567 ( 0.000027 0.000035 0.000026 ) -0.016077 0.064813 0.012944 ( 0.000033 0.000043 0.000031 ) -0.003510 -0.014155 0.066480 ( 0.000024 0.000031 0.000023 ) M - matrix: 0.004638 0.000013 -0.000007 ( 0.000004 0.000003 0.000002 ) 0.000013 0.004633 -0.000002 ( 0.000003 0.000006 0.000003 ) -0.000007 -0.000002 0.004630 ( 0.000002 0.000003 0.000003 ) unit cell: 10.416(4) 10.421(6) 10.424(4) 89.97(4) 89.91(3) 90.16(4) V = 1131.4(9) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 UB fit with 215 obs out of 238 (total:238,skipped:0) (90.34%) UB - matrix: 0.066084 0.015282 0.006514 ( 0.000025 0.000034 0.000026 ) -0.016242 0.064813 0.012906 ( 0.000028 0.000037 0.000029 ) -0.003399 -0.014131 0.066459 ( 0.000021 0.000028 0.000022 ) M - matrix: 0.004642 0.000005 -0.000005 ( 0.000003 0.000003 0.000002 ) 0.000005 0.004634 -0.000003 ( 0.000003 0.000005 0.000003 ) -0.000005 -0.000003 0.004626 ( 0.000002 0.000003 0.000003 ) unit cell: 10.410(4) 10.420(5) 10.429(3) 89.96(3) 89.94(3) 90.06(4) V = 1131.2(8) OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 OTKP changes: 94 1 1 1 Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066068 0.015279 0.006507 ( 0.000023 0.000031 0.000024 ) -0.016353 0.064775 0.012903 ( 0.000026 0.000036 0.000028 ) -0.003378 -0.014136 0.066452 ( 0.000022 0.000030 0.000024 ) M - matrix: 0.004644 -0.000002 -0.000006 ( 0.000003 0.000003 0.000002 ) -0.000002 0.004629 -0.000004 ( 0.000003 0.000005 0.000003 ) -0.000006 -0.000004 0.004625 ( 0.000002 0.000003 0.000003 ) UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) unit cell: 10.409(4) 10.425(5) 10.430(4) 89.95(3) 89.93(3) 89.97(3) V = 1131.8(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 221 obs out of 238 (total:238,skipped:0) (92.86%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 229 peaks identified as outliers and rejected 229 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 229 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 229 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.39 | 23 | 0.876 ( 0.100) | 0.884 ( 0.132) | 0.997 ( 0.519) | 2.38- 1.76 | 23 | 0.894 ( 0.109) | 0.910 ( 0.154) | 0.921 ( 0.275) | 1.76- 1.58 | 23 | 0.890 ( 0.112) | 0.908 ( 0.156) | 0.804 ( 0.259) | 1.57- 1.35 | 23 | 0.943 ( 0.089) | 0.975 ( 0.133) | 0.782 ( 0.389) | 1.35- 1.16 | 23 | 0.951 ( 0.069) | 0.963 ( 0.076) | 1.014 ( 0.478) | 1.16- 1.00 | 23 | 0.957 ( 0.087) | 0.974 ( 0.121) | 0.876 ( 0.297) | 1.00- 0.88 | 23 | 0.989 ( 0.063) | 0.998 ( 0.078) | 1.042 ( 0.389) | 0.88- 0.79 | 23 | 0.986 ( 0.043) | 0.974 ( 0.127) | 1.036 ( 0.389) | 0.79- 0.69 | 23 | 0.964 ( 0.047) | 0.916 ( 0.088) | 1.251 ( 0.494) | 0.69- 0.63 | 22 | 0.933 ( 0.050) | 0.848 ( 0.069) | 1.282 ( 0.443) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 229 | 0.938 ( 0.089) | 0.936 ( 0.126) | 0.999 ( 0.433) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) UB - matrix: 0.066173 0.015305 0.006655 ( 0.000018 0.000024 0.000020 ) -0.016448 0.064787 0.012868 ( 0.000014 0.000019 0.000016 ) -0.003393 -0.014234 0.066455 ( 0.000012 0.000017 0.000014 ) M - matrix: 0.004661 -0.000005 0.000003 ( 0.000002 0.000002 0.000002 ) -0.000005 0.004634 -0.000010 ( 0.000002 0.000003 0.000002 ) 0.000003 -0.000010 0.004626 ( 0.000002 0.000002 0.000002 ) unit cell: 10.389(3) 10.419(3) 10.429(2) 89.87(2) 90.04(2) 89.94(2) V = 1128.9(5) OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 OTKP changes: 229 1 1 1 No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.156) HKL list info: 1313 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004642 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004618 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004633 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066060 0.015209 0.006553 ( 0.000013 0.000017 0.000015 ) -0.016315 0.064696 0.012956 ( 0.000012 0.000016 0.000013 ) -0.003377 -0.014170 0.066502 ( 0.000010 0.000014 0.000012 ) M - matrix: 0.004633 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004633 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004633 ( 0.000000 0.000000 0.000000 ) UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) unit cell: 10.411(2) 10.438(2) 10.4204(18) 89.945(16) 89.962(15) 89.964(17) V = 1132.4(4) unit cell: 10.4232(5) 10.4232(5) 10.4232(5) 90.0 90.0 90.0 V = 1132.40(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 229 obs out of 229 (total:229,skipped:0) (100.00%) 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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.rpb 0 of 222 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" 222 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4.tabbin file 222 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 2.39 | 22 | 0.882 ( 0.101) | 0.891 ( 0.127) | 0.921 ( 0.461) | 2.39- 1.84 | 22 | 0.903 ( 0.107) | 0.920 ( 0.157) | 0.921 ( 0.277) | 1.76- 1.59 | 22 | 0.877 ( 0.115) | 0.887 ( 0.167) | 0.786 ( 0.224) | 1.59- 1.36 | 22 | 0.957 ( 0.074) | 0.988 ( 0.115) | 0.886 ( 0.459) | 1.36- 1.19 | 22 | 0.927 ( 0.082) | 0.951 ( 0.107) | 0.807 ( 0.452) | 1.19- 1.01 | 22 | 0.970 ( 0.081) | 0.999 ( 0.117) | 0.890 ( 0.367) | 1.01- 0.88 | 22 | 0.977 ( 0.064) | 0.989 ( 0.076) | 1.041 ( 0.396) | 0.88- 0.79 | 22 | 0.986 ( 0.045) | 0.983 ( 0.130) | 1.012 ( 0.380) | 0.79- 0.69 | 22 | 0.971 ( 0.045) | 0.933 ( 0.091) | 1.199 ( 0.476) | 0.69- 0.63 | 24 | 0.932 ( 0.048) | 0.851 ( 0.074) | 1.272 ( 0.439) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.97- 0.63 | 222 | 0.938 ( 0.089) | 0.938 ( 0.129) | 0.976 ( 0.430) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) UB fit with 239 obs out of 301 (total:302,skipped:1) (79.40%) UB - matrix: 0.066021 0.015265 0.006428 ( 0.000038 0.000029 0.000025 ) -0.016248 0.064745 0.013273 ( 0.000038 0.000029 0.000026 ) -0.003288 -0.014501 0.066429 ( 0.000043 0.000033 0.000029 ) M - matrix: 0.004634 0.000003 -0.000010 ( 0.000005 0.000003 0.000003 ) 0.000003 0.004635 -0.000006 ( 0.000003 0.000004 0.000003 ) -0.000010 -0.000006 0.004630 ( 0.000003 0.000003 0.000004 ) unit cell: 10.420(6) 10.418(5) 10.424(4) 89.93(4) 89.88(4) 90.04(4) V = 1131.6(9) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) 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 Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066001 0.015413 0.006308 ( 0.000032 0.000025 0.000024 ) -0.016359 0.064725 0.013344 ( 0.000030 0.000023 0.000022 ) -0.002915 -0.014619 0.066407 ( 0.000028 0.000022 0.000021 ) M - matrix: 0.004632 0.000001 0.000004 ( 0.000004 0.000003 0.000003 ) 0.000001 0.004641 -0.000010 ( 0.000003 0.000003 0.000002 ) 0.000004 -0.000010 0.004628 ( 0.000003 0.000002 0.000003 ) UB fit with 274 obs out of 301 (total:302,skipped:1) (91.03%) unit cell: 10.422(5) 10.412(4) 10.427(3) 89.88(3) 90.06(3) 90.01(3) V = 1131.4(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 275 obs out of 301 (total:302,skipped:1) (91.36%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 278 peaks identified as outliers and rejected 278 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 278 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 278 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 2.13 | 28 | 0.894 ( 0.102) | 0.904 ( 0.131) | 0.866 ( 0.306) | 2.13- 1.75 | 28 | 0.901 ( 0.127) | 0.984 ( 0.362) | 0.979 ( 0.568) | 1.75- 1.56 | 28 | 0.955 ( 0.112) | 0.968 ( 0.143) | 0.963 ( 0.405) | 1.56- 1.35 | 28 | 0.959 ( 0.096) | 0.969 ( 0.157) | 0.837 ( 0.390) | 1.35- 1.19 | 28 | 0.938 ( 0.097) | 0.973 ( 0.155) | 0.714 ( 0.265) | 1.19- 1.06 | 28 | 0.984 ( 0.065) | 1.017 ( 0.109) | 0.883 ( 0.347) | 1.06- 0.92 | 28 | 1.006 ( 0.077) | 1.060 ( 0.122) | 0.951 ( 0.373) | 0.91- 0.87 | 28 | 1.006 ( 0.063) | 1.002 ( 0.121) | 1.080 ( 0.336) | 0.87- 0.73 | 28 | 1.038 ( 0.052) | 1.012 ( 0.133) | 1.210 ( 0.460) | 0.73- 0.63 | 26 | 1.004 ( 0.040) | 1.020 ( 0.127) | 1.061 ( 0.360) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.94- 0.63 | 278 | 0.968 ( 0.098) | 0.991 ( 0.176) | 0.954 ( 0.412) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) UB - matrix: 0.066020 0.015434 0.006403 ( 0.000019 0.000014 0.000015 ) -0.016416 0.064853 0.013481 ( 0.000022 0.000017 0.000018 ) -0.002784 -0.014649 0.066450 ( 0.000018 0.000013 0.000014 ) M - matrix: 0.004636 -0.000005 0.000016 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004659 -0.000000 ( 0.000002 0.000002 0.000001 ) 0.000016 -0.000000 0.004638 ( 0.000002 0.000001 0.000002 ) unit cell: 10.418(3) 10.392(3) 10.415(2) 89.997(19) 90.203(19) 89.94(2) V = 1127.5(5) OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 OTKP changes: 277 1 1 1 No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.156) HKL list info: 1314 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004624 -0.000004 0.000007 ( 0.000002 0.000001 0.000001 ) -0.000004 0.004643 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000007 -0.000009 0.004636 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.065952 0.015338 0.006295 ( 0.000016 0.000012 0.000013 ) -0.016328 0.064754 0.013399 ( 0.000018 0.000014 0.000014 ) -0.002848 -0.014645 0.066458 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) unit cell: 10.430(2) 10.410(2) 10.4177(19) 89.888(16) 90.088(17) 89.950(18) V = 1131.1(4) unit cell: 10.4193(6) 10.4193(6) 10.4193(6) 90.0 90.0 90.0 V = 1131.13(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 278 (total:278,skipped:0) (99.64%) 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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.rpb 0 of 271 peaks identified as outliers and rejected 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" 271 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5.tabbin file 271 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 2.12 | 27 | 0.894 ( 0.101) | 0.908 ( 0.136) | 0.840 ( 0.298) | 2.12- 1.76 | 27 | 0.919 ( 0.126) | 1.028 ( 0.462) | 0.961 ( 0.470) | 1.75- 1.50 | 27 | 0.977 ( 0.114) | 1.004 ( 0.144) | 1.014 ( 0.419) | 1.50- 1.35 | 27 | 0.958 ( 0.091) | 0.972 ( 0.157) | 0.817 ( 0.387) | 1.35- 1.19 | 27 | 0.940 ( 0.104) | 0.969 ( 0.154) | 0.724 ( 0.286) | 1.16- 1.06 | 27 | 0.985 ( 0.067) | 1.028 ( 0.102) | 0.895 ( 0.342) | 1.06- 0.92 | 27 | 1.004 ( 0.076) | 1.059 ( 0.128) | 0.985 ( 0.375) | 0.91- 0.87 | 27 | 1.008 ( 0.060) | 1.002 ( 0.108) | 1.166 ( 0.421) | 0.87- 0.73 | 27 | 1.041 ( 0.054) | 1.026 ( 0.133) | 1.208 ( 0.469) | 0.73- 0.63 | 28 | 1.003 ( 0.040) | 1.017 ( 0.123) | 1.056 ( 0.350) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.98- 0.63 | 271 | 0.973 ( 0.097) | 1.001 ( 0.197) | 0.967 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) UB fit with 126 obs out of 199 (total:199,skipped:0) (63.32%) UB - matrix: 0.066110 0.015190 0.006395 ( 0.000069 0.000079 0.000061 ) -0.016243 0.064649 0.013093 ( 0.000055 0.000063 0.000049 ) -0.003827 -0.013998 0.066465 ( 0.000068 0.000077 0.000060 ) M - matrix: 0.004649 0.000008 -0.000044 ( 0.000009 0.000007 0.000006 ) 0.000008 0.004606 0.000013 ( 0.000007 0.000009 0.000006 ) -0.000044 0.000013 0.004630 ( 0.000006 0.000006 0.000008 ) unit cell: 10.403(11) 10.451(10) 10.425(9) 90.16(8) 89.45(8) 90.10(8) V = 1133(2) OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 OTKP changes: 77 1 1 1 UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 OTKP changes: 82 1 1 1 Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.156) HKL list info: 1283 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.065882 0.015582 0.006291 ( 0.000039 0.000033 0.000035 ) -0.016480 0.064498 0.013033 ( 0.000034 0.000029 0.000031 ) -0.002797 -0.014298 0.066468 ( 0.000024 0.000020 0.000022 ) M - matrix: 0.004620 0.000004 0.000014 ( 0.000005 0.000003 0.000003 ) 0.000004 0.004607 -0.000012 ( 0.000003 0.000004 0.000003 ) 0.000014 -0.000012 0.004627 ( 0.000003 0.000003 0.000003 ) UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) unit cell: 10.436(6) 10.450(5) 10.427(3) 89.85(3) 90.17(4) 90.05(4) V = 1137.1(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 185 obs out of 199 (total:199,skipped:0) (92.96%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 192 peaks identified as outliers and rejected 192 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 192 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 192 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 2.97 | 19 | 0.842 ( 0.116) | 0.844 ( 0.171) | 0.956 ( 0.449) | 2.63- 1.84 | 19 | 0.822 ( 0.111) | 0.843 ( 0.187) | 0.847 ( 0.504) | 1.84- 1.59 | 19 | 0.842 ( 0.108) | 0.837 ( 0.164) | 0.836 ( 0.354) | 1.59- 1.36 | 19 | 0.936 ( 0.096) | 0.973 ( 0.144) | 0.805 ( 0.268) | 1.36- 1.20 | 19 | 0.950 ( 0.102) | 0.972 ( 0.160) | 0.845 ( 0.330) | 1.20- 1.01 | 19 | 0.995 ( 0.078) | 1.010 ( 0.137) | 1.101 ( 0.434) | 1.01- 0.88 | 19 | 0.998 ( 0.085) | 1.016 ( 0.121) | 1.030 ( 0.364) | 0.88- 0.79 | 19 | 1.037 ( 0.059) | 1.056 ( 0.123) | 0.938 ( 0.316) | 0.79- 0.72 | 19 | 1.031 ( 0.054) | 0.994 ( 0.144) | 1.279 ( 0.526) | 0.70- 0.63 | 21 | 0.975 ( 0.052) | 0.883 ( 0.059) | 1.164 ( 0.415) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.03- 0.63 | 192 | 0.943 ( 0.117) | 0.942 ( 0.164) | 0.982 ( 0.432) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) UB - matrix: 0.065810 0.015591 0.006262 ( 0.000023 0.000019 0.000022 ) -0.016403 0.064531 0.013131 ( 0.000023 0.000020 0.000022 ) -0.002751 -0.014148 0.066421 ( 0.000026 0.000022 0.000025 ) M - matrix: 0.004608 0.000006 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000006 0.004607 0.000005 ( 0.000002 0.000003 0.000002 ) 0.000014 0.000005 0.004623 ( 0.000002 0.000002 0.000003 ) unit cell: 10.450(3) 10.450(3) 10.432(4) 90.07(3) 90.17(3) 90.08(3) V = 1139.1(6) OTKP changes: 192 1 1 1 OTKP changes: 192 1 1 1 No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.027) HKL list info: 1279 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004641 0.000007 0.000014 ( 0.000003 0.000002 0.000002 ) 0.000007 0.004635 -0.000012 ( 0.000002 0.000002 0.000002 ) 0.000014 -0.000012 0.004648 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066053 0.015570 0.006349 ( 0.000019 0.000016 0.000018 ) -0.016418 0.064700 0.013078 ( 0.000022 0.000019 0.000021 ) -0.002863 -0.014365 0.066610 ( 0.000014 0.000012 0.000013 ) M - matrix: 0.004643 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004643 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004643 ( 0.000000 0.000000 0.000001 ) UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) unit cell: 10.412(3) 10.419(3) 10.404(2) 89.85(2) 90.172(19) 90.09(2) V = 1128.6(5) unit cell: 10.4115(6) 10.4115(6) 10.4115(6) 90.0 90.0 90.0 V = 1128.59(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 192 obs out of 192 (total:192,skipped:0) (100.00%) 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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.rpb 0 of 190 peaks identified as outliers and rejected 190 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" 190 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6.tabbin file 190 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 3.00 | 19 | 0.846 ( 0.114) | 0.847 ( 0.168) | 0.873 ( 0.501) | 2.99- 2.00 | 19 | 0.802 ( 0.108) | 0.800 ( 0.186) | 0.843 ( 0.452) | 1.84- 1.59 | 19 | 0.842 ( 0.097) | 0.828 ( 0.155) | 0.880 ( 0.351) | 1.59- 1.36 | 19 | 0.948 ( 0.083) | 0.983 ( 0.140) | 0.851 ( 0.258) | 1.36- 1.19 | 19 | 0.950 ( 0.094) | 0.960 ( 0.152) | 0.768 ( 0.211) | 1.19- 1.00 | 19 | 1.018 ( 0.060) | 1.041 ( 0.127) | 1.085 ( 0.364) | 1.00- 0.88 | 19 | 1.010 ( 0.085) | 1.031 ( 0.121) | 1.045 ( 0.373) | 0.88- 0.78 | 19 | 1.033 ( 0.056) | 1.044 ( 0.117) | 0.953 ( 0.322) | 0.78- 0.69 | 19 | 1.031 ( 0.055) | 1.004 ( 0.165) | 1.278 ( 0.531) | 0.69- 0.63 | 19 | 0.970 ( 0.050) | 0.876 ( 0.055) | 1.127 ( 0.364) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 190 | 0.945 ( 0.116) | 0.942 ( 0.169) | 0.970 ( 0.413) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) UB fit with 62 obs out of 106 (total:106,skipped:0) (58.49%) UB - matrix: 0.065950 0.015170 0.006478 ( 0.000215 0.000078 0.000070 ) -0.016096 0.064743 0.013375 ( 0.000122 0.000044 0.000040 ) -0.002971 -0.014337 0.066487 ( 0.000185 0.000067 0.000060 ) M - matrix: 0.004617 0.000001 0.000014 ( 0.000029 0.000010 0.000013 ) 0.000001 0.004627 0.000011 ( 0.000010 0.000007 0.000005 ) 0.000014 0.000011 0.004641 ( 0.000013 0.000005 0.000008 ) unit cell: 10.44(3) 10.427(9) 10.411(10) 90.14(8) 90.18(16) 90.01(13) V = 1133(4) OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 OTKP changes: 39 1 1 1 UB - matrix: 0.066110 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) UB - matrix: 0.066109 0.015287 0.006079 ( 0.000116 0.000057 0.000055 ) -0.016361 0.064607 0.013536 ( 0.000062 0.000030 0.000029 ) -0.002217 -0.014474 0.066375 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004643 -0.000014 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000014 0.004617 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000007 0.004626 ( 0.000007 0.000003 0.000005 ) unit cell: 10.410(17) 10.439(6) 10.429(6) 90.08(5) 90.41(8) 89.82(8) V = 1133(2) OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 OTKP changes: 40 1 1 1 UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: 0.066101 0.015294 0.006078 ( 0.000116 0.000057 0.000055 ) -0.016352 0.064596 0.013517 ( 0.000061 0.000030 0.000029 ) -0.002219 -0.014476 0.066370 ( 0.000081 0.000040 0.000038 ) M - matrix: 0.004642 -0.000013 0.000033 ( 0.000015 0.000006 0.000007 ) -0.000013 0.004616 0.000005 ( 0.000006 0.000004 0.000003 ) 0.000033 0.000005 0.004625 ( 0.000007 0.000003 0.000005 ) UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) unit cell: 10.411(17) 10.440(6) 10.430(6) 90.07(5) 90.41(8) 89.84(8) V = 1134(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 96 obs out of 106 (total:106,skipped:0) (90.57%) 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= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 100 peaks identified as outliers and rejected 100 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 100 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 100 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 2.37 | 10 | 0.824 ( 0.107) | 0.789 ( 0.168) | 0.948 ( 0.526) | 2.13- 1.65 | 10 | 0.887 ( 0.099) | 0.902 ( 0.146) | 0.800 ( 0.370) | 1.64- 1.46 | 10 | 0.917 ( 0.142) | 0.896 ( 0.234) | 0.948 ( 0.416) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.161) | 1.038 ( 0.459) | 1.23- 1.11 | 10 | 1.014 ( 0.089) | 1.022 ( 0.172) | 1.004 ( 0.500) | 1.11- 1.00 | 10 | 0.988 ( 0.107) | 1.011 ( 0.206) | 0.971 ( 0.392) | 1.00- 0.89 | 10 | 1.016 ( 0.106) | 1.093 ( 0.173) | 0.829 ( 0.141) | 0.89- 0.86 | 10 | 0.995 ( 0.094) | 1.038 ( 0.093) | 1.245 ( 0.487) | 0.82- 0.73 | 10 | 1.072 ( 0.046) | 1.130 ( 0.142) | 0.868 ( 0.108) | 0.72- 0.64 | 10 | 1.031 ( 0.064) | 1.069 ( 0.171) | 1.233 ( 0.765) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.16- 0.64 | 100 | 0.972 ( 0.121) | 0.995 ( 0.197) | 0.988 ( 0.476) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) UB - matrix: 0.065966 0.015448 0.005965 ( 0.000053 0.000028 0.000028 ) -0.016426 0.064502 0.013369 ( 0.000054 0.000029 0.000028 ) -0.002418 -0.014553 0.066425 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004627 -0.000005 0.000013 ( 0.000007 0.000004 0.000003 ) -0.000005 0.004611 -0.000012 ( 0.000004 0.000004 0.000002 ) 0.000013 -0.000012 0.004627 ( 0.000003 0.000002 0.000002 ) unit cell: 10.427(8) 10.446(5) 10.428(3) 89.85(3) 90.16(4) 89.93(5) V = 1136(1) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.156) HKL list info: 694 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004639 -0.000017 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000017 0.004623 -0.000002 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000002 0.004633 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066035 0.015377 0.005982 ( 0.000051 0.000027 0.000027 ) -0.016508 0.064612 0.013507 ( 0.000029 0.000016 0.000015 ) -0.002385 -0.014549 0.066440 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004630 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004630 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004630 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 10.414(7) 10.432(3) 10.421(3) 89.98(2) 90.17(3) 89.80(3) V = 1132.2(9) unit cell: 10.4226(9) 10.4226(9) 10.4226(9) 90.0 90.0 90.0 V = 1132.21(18) 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! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -24.51 ka= 56.89 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=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb 0 of 101 peaks identified as outliers and rejected 101 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" 101 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7.tabbin file 101 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 2.38 | 10 | 0.825 ( 0.107) | 0.790 ( 0.169) | 1.019 ( 0.527) | 2.13- 1.64 | 10 | 0.860 ( 0.122) | 0.859 ( 0.190) | 0.860 ( 0.389) | 1.64- 1.46 | 10 | 0.944 ( 0.113) | 0.943 ( 0.190) | 0.940 ( 0.402) | 1.36- 1.23 | 10 | 0.974 ( 0.094) | 0.993 ( 0.160) | 1.023 ( 0.449) | 1.23- 1.11 | 10 | 1.002 ( 0.107) | 0.995 ( 0.210) | 0.997 ( 0.506) | 1.09- 1.00 | 10 | 1.034 ( 0.082) | 1.115 ( 0.140) | 0.886 ( 0.284) | 0.97- 0.88 | 10 | 0.989 ( 0.091) | 1.159 ( 0.229) | 0.740 ( 0.286) | 0.88- 0.86 | 10 | 1.009 ( 0.084) | 1.059 ( 0.096) | 1.119 ( 0.453) | 0.82- 0.73 | 10 | 1.071 ( 0.046) | 1.128 ( 0.142) | 0.868 ( 0.110) | 0.72- 0.63 | 11 | 1.023 ( 0.066) | 1.042 ( 0.168) | 1.108 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 3.14- 0.63 | 101 | 0.974 ( 0.119) | 1.009 ( 0.206) | 0.958 ( 0.416) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 8 *** 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_75.img BACKGROUND INFO: Creating background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_75.img BACKGROUND INFO: Creating background info file D:\Data\xs2212a\tmp\xs2212a_back_8_75.rpb PROFFITPEAK info: 421 peaks in the peak location table UB fit with 140 obs out of 243 (total:243,skipped:0) (57.61%) UB - matrix: 0.065888 0.015314 0.006403 ( 0.000080 0.000043 0.000047 ) -0.016419 0.064733 0.013289 ( 0.000068 0.000037 0.000040 ) -0.003158 -0.014335 0.066501 ( 0.000083 0.000045 0.000049 ) M - matrix: 0.004621 -0.000009 -0.000006 ( 0.000011 0.000006 0.000006 ) -0.000009 0.004630 0.000005 ( 0.000006 0.000005 0.000004 ) -0.000006 0.000005 0.004640 ( 0.000006 0.000004 0.000007 ) unit cell: 10.434(12) 10.424(6) 10.413(7) 90.06(5) 89.92(8) 89.89(7) V = 1133(2) UB fit with 140 obs out of 243 (total:243,skipped:0) (57.61%) UB - matrix: 0.065888 0.015314 0.006403 ( 0.000080 0.000043 0.000047 ) -0.016419 0.064733 0.013289 ( 0.000068 0.000037 0.000040 ) -0.003158 -0.014335 0.066501 ( 0.000083 0.000045 0.000049 ) M - matrix: 0.004621 -0.000009 -0.000006 ( 0.000011 0.000006 0.000006 ) -0.000009 0.004630 0.000005 ( 0.000006 0.000005 0.000004 ) -0.000006 0.000005 0.004640 ( 0.000006 0.000004 0.000007 ) unit cell: 10.434(12) 10.424(6) 10.413(7) 90.06(5) 89.92(8) 89.89(7) V = 1133(2) OTKP changes: 87 1 1 1 OTKP changes: 87 1 1 1 OTKP changes: 87 1 1 1 No constraint UB - matrix: 0.065770 0.015574 0.005959 ( 0.000046 0.000028 0.000036 ) -0.016610 0.064573 0.013483 ( 0.000033 0.000021 0.000026 ) -0.002296 -0.014594 0.066436 ( 0.000030 0.000018 0.000024 ) M - matrix: 0.004607 -0.000015 0.000015 ( 0.000006 0.000003 0.000003 ) -0.000015 0.004625 -0.000006 ( 0.000003 0.000003 0.000002 ) 0.000015 -0.000006 0.004631 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.065770 0.015574 0.005959 ( 0.000046 0.000028 0.000036 ) -0.016610 0.064573 0.013483 ( 0.000033 0.000021 0.000026 ) -0.002296 -0.014594 0.066436 ( 0.000030 0.000018 0.000024 ) M - matrix: 0.004621 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004621 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004621 ( 0.000000 0.000000 0.000001 ) UB fit with 223 obs out of 243 (total:243,skipped:0) (91.77%) unit cell: 10.450(7) 10.430(3) 10.423(4) 89.93(3) 90.19(4) 89.82(4) V = 1136.0(9) unit cell: 10.4343(14) 10.4343(14) 10.4343(14) 90.0 90.0 90.0 V = 1136.0(3) UB fit with 223 obs out of 243 (total:243,skipped:0) (91.77%) UB - matrix: 0.065770 0.015574 0.005959 ( 0.000046 0.000028 0.000036 ) -0.016610 0.064573 0.013483 ( 0.000033 0.000021 0.000026 ) -0.002296 -0.014594 0.066436 ( 0.000030 0.000018 0.000024 ) M - matrix: 0.004607 -0.000015 0.000015 ( 0.000006 0.000003 0.000003 ) -0.000015 0.004625 -0.000006 ( 0.000003 0.000003 0.000002 ) 0.000015 -0.000006 0.004631 ( 0.000003 0.000002 0.000003 ) unit cell: 10.450(7) 10.430(3) 10.423(4) 89.93(3) 90.19(4) 89.82(4) V = 1136.0(9) OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 243 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_8" Run 8 Omega scan: (-49.000 - 50.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.156) HKL list info: 1264 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065770 0.015574 0.005959 ( 0.000046 0.000028 0.000036 ) -0.016610 0.064573 0.013483 ( 0.000033 0.000021 0.000026 ) -0.002296 -0.014594 0.066436 ( 0.000030 0.000018 0.000024 ) M - matrix: 0.004607 -0.000015 0.000015 ( 0.000006 0.000003 0.000003 ) -0.000015 0.004625 -0.000006 ( 0.000003 0.000003 0.000002 ) 0.000015 -0.000006 0.004631 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.065770 0.015574 0.005959 ( 0.000046 0.000028 0.000036 ) -0.016610 0.064573 0.013483 ( 0.000033 0.000021 0.000026 ) -0.002296 -0.014594 0.066436 ( 0.000030 0.000018 0.000024 ) M - matrix: 0.004621 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004621 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004621 ( 0.000000 0.000000 0.000001 ) UB fit with 223 obs out of 243 (total:243,skipped:0) (91.77%) unit cell: 10.450(7) 10.430(3) 10.423(4) 89.93(3) 90.19(4) 89.82(4) V = 1136.0(9) unit cell: 10.4343(14) 10.4343(14) 10.4343(14) 90.0 90.0 90.0 V = 1136.0(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 223 obs out of 243 (total:243,skipped:0) (91.77%) 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= -24.51 ka= 37.89 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=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_75.rpb 0 of 225 peaks identified as outliers and rejected 225 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" 225 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8.tabbin file 225 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.93- 2.37 | 23 | 0.829 ( 0.091) | 0.803 ( 0.161) | 0.891 ( 0.469) | 2.14- 1.65 | 23 | 0.874 ( 0.111) | 1.028 ( 0.697) | 0.749 ( 0.417) | 1.65- 1.36 | 23 | 0.966 ( 0.110) | 0.991 ( 0.181) | 0.911 ( 0.426) | 1.36- 1.20 | 23 | 0.971 ( 0.084) | 1.008 ( 0.159) | 0.736 ( 0.336) | 1.20- 1.09 | 23 | 1.024 ( 0.090) | 1.026 ( 0.176) | 1.007 ( 0.454) | 1.09- 1.00 | 23 | 1.033 ( 0.071) | 1.093 ( 0.136) | 0.887 ( 0.349) | 1.00- 0.88 | 23 | 0.990 ( 0.124) | 1.044 ( 0.141) | 1.013 ( 0.375) | 0.88- 0.78 | 23 | 1.049 ( 0.063) | 1.079 ( 0.136) | 1.127 ( 0.482) | 0.78- 0.69 | 23 | 1.026 ( 0.058) | 1.018 ( 0.136) | 1.252 ( 0.507) | 0.69- 0.63 | 18 | 1.024 ( 0.055) | 0.936 ( 0.097) | 1.410 ( 0.546) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 5.93- 0.63 | 225 | 0.978 ( 0.113) | 1.004 ( 0.276) | 0.989 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" UB fit with 225 obs out of 225 (total:225,skipped:0) (100.00%) UB - matrix: 0.065801 0.015639 0.005801 ( 0.000025 0.000017 0.000021 ) -0.016632 0.064439 0.013434 ( 0.000026 0.000017 0.000021 ) -0.002326 -0.014507 0.066515 ( 0.000017 0.000012 0.000015 ) M - matrix: 0.004612 -0.000009 0.000004 ( 0.000003 0.000002 0.000002 ) -0.000009 0.004607 -0.000009 ( 0.000002 0.000002 0.000002 ) 0.000004 -0.000009 0.004638 ( 0.000002 0.000002 0.000002 ) unit cell: 10.445(4) 10.450(3) 10.415(2) 89.89(2) 90.04(2) 89.89(3) V = 1136.7(6) OTKP changes: 225 1 1 1 OTKP changes: 225 1 1 1 OTKP changes: 225 1 1 1 No constraint UB - matrix: 0.065881 0.015622 0.005896 ( 0.000021 0.000014 0.000018 ) -0.016656 0.064600 0.013515 ( 0.000019 0.000013 0.000016 ) -0.002271 -0.014584 0.066510 ( 0.000016 0.000011 0.000013 ) M - matrix: 0.004623 -0.000014 0.000012 ( 0.000003 0.000002 0.000002 ) -0.000014 0.004630 -0.000005 ( 0.000002 0.000002 0.000001 ) 0.000012 -0.000005 0.004641 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.065881 0.015622 0.005896 ( 0.000021 0.000014 0.000018 ) -0.016656 0.064600 0.013515 ( 0.000019 0.000013 0.000016 ) -0.002271 -0.014584 0.066510 ( 0.000016 0.000011 0.000013 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 224 obs out of 225 (total:225,skipped:0) (99.56%) unit cell: 10.432(3) 10.424(2) 10.412(2) 89.941(17) 90.15(2) 89.83(2) V = 1132.3(5) unit cell: 10.4227(7) 10.4227(7) 10.4227(7) 90.0 90.0 90.0 V = 1132.25(12) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-49.000 - 50.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.156) HKL list info: 1259 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065881 0.015622 0.005896 ( 0.000021 0.000014 0.000018 ) -0.016656 0.064600 0.013515 ( 0.000019 0.000013 0.000016 ) -0.002271 -0.014584 0.066510 ( 0.000016 0.000011 0.000013 ) M - matrix: 0.004623 -0.000014 0.000012 ( 0.000003 0.000002 0.000002 ) -0.000014 0.004630 -0.000005 ( 0.000002 0.000002 0.000001 ) 0.000012 -0.000005 0.004641 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.065881 0.015622 0.005896 ( 0.000021 0.000014 0.000018 ) -0.016656 0.064600 0.013515 ( 0.000019 0.000013 0.000016 ) -0.002271 -0.014584 0.066510 ( 0.000016 0.000011 0.000013 ) M - matrix: 0.004632 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004632 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004632 ( 0.000000 0.000000 0.000001 ) UB fit with 224 obs out of 225 (total:225,skipped:0) (99.56%) unit cell: 10.432(3) 10.424(2) 10.412(2) 89.941(17) 90.15(2) 89.83(2) V = 1132.3(5) unit cell: 10.4227(7) 10.4227(7) 10.4227(7) 90.0 90.0 90.0 V = 1132.25(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 224 obs out of 225 (total:225,skipped:0) (99.56%) 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= -24.51 ka= 37.89 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=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_75.rpb 0 of 224 peaks identified as outliers and rejected 224 peaks stored in the peak table Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" 224 peaks saved into the D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8.tabbin file 224 profiles saved into the file D:\Data\xs2212a\tmp\xs2212a_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) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 2.38 | 22 | 0.846 ( 0.092) | 0.830 ( 0.160) | 0.902 ( 0.551) | 2.38- 1.76 | 22 | 0.839 ( 0.112) | 0.839 ( 0.188) | 0.714 ( 0.202) | 1.75- 1.50 | 22 | 1.017 ( 0.362) | 1.073 ( 0.490) | 1.114 ( 1.485) | 1.46- 1.23 | 22 | 1.000 ( 0.083) | 1.055 ( 0.133) | 0.736 ( 0.256) | 1.23- 1.11 | 22 | 0.992 ( 0.102) | 1.010 ( 0.167) | 0.973 ( 0.463) | 1.11- 1.01 | 22 | 1.014 ( 0.088) | 1.045 ( 0.164) | 0.953 ( 0.346) | 1.01- 0.89 | 22 | 1.033 ( 0.072) | 1.061 ( 0.118) | 1.047 ( 0.335) | 0.88- 0.79 | 22 | 1.039 ( 0.080) | 1.081 ( 0.116) | 1.129 ( 0.401) | 0.79- 0.72 | 22 | 1.038 ( 0.051) | 1.028 ( 0.127) | 1.337 ( 0.547) | 0.71- 0.63 | 26 | 1.016 ( 0.059) | 0.962 ( 0.123) | 1.251 ( 0.494) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 6.01- 0.63 | 224 | 0.984 ( 0.156) | 0.998 ( 0.225) | 1.020 ( 0.641) | 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) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-10.6 | 172 | 1.009 ( 0.130) | 1.065 ( 0.178) | 1.144 ( 0.692) | 10.6-15.3 | 172 | 1.014 ( 0.161) | 1.060 ( 0.078) | 1.148 ( 0.908) | 15.4-19.6 | 172 | 0.987 ( 0.064) | 1.041 ( 0.097) | 1.036 ( 0.441) | 19.6-23.8 | 172 | 0.978 ( 0.068) | 1.019 ( 0.090) | 0.936 ( 0.404) | 23.8-27.8 | 172 | 0.980 ( 0.072) | 1.021 ( 0.117) | 0.964 ( 0.446) | 27.9-32.7 | 172 | 0.953 ( 0.088) | 0.972 ( 0.121) | 0.952 ( 0.457) | 32.7-36.3 | 172 | 0.924 ( 0.149) | 0.915 ( 0.151) | 1.056 ( 0.626) | 36.4-39.0 | 172 | 0.892 ( 0.109) | 0.878 ( 0.233) | 1.023 ( 0.489) | 39.0-42.0 | 172 | 0.896 ( 0.112) | 0.849 ( 0.166) | 0.981 ( 0.440) | 42.0-50.2 | 173 | 0.877 ( 0.129) | 0.799 ( 0.150) | 0.927 ( 0.431) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.2 | 1721 | 0.951 ( 0.123) | 0.962 ( 0.171) | 1.017 ( 0.560) | Fitted profile normalization line parameters e1 dimension: a=-0.0034 b=1.15 e2 dimension: a=-0.0069 b=1.25 e3 dimension: a=-0.0006 b=1.13 Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_peakhunt_8" Writing tabbin file: "D:\Data\xs2212a\xs2212a_peakhunt" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 9679 lp-corr: 5011 Maximum peak integral for reflections I/sig<= 100 - raw: 468227 lp-corr: 385993 Maximum peak integral for reflections I/sig<= 10000 - raw: 12008066 lp-corr: 1563362 PROFFITPEAK - Finished at Wed Aug 21 15:26:06 2019 PROFFITMAIN - Started at Wed Aug 21 15:26:06 2019 OTKP changes: 1327 2 7 8 OTKP changes: 1327 2 7 8 OTKP changes: 1327 2 7 8 No constraint UB - matrix: 0.066186 0.015243 0.006615 ( 0.000012 0.000012 0.000012 ) -0.016280 0.064853 0.013216 ( 0.000010 0.000010 0.000011 ) -0.003427 -0.014389 0.066491 ( 0.000014 0.000014 0.000014 ) M - matrix: 0.004657 0.000002 -0.000005 ( 0.000002 0.000001 0.000001 ) 0.000002 0.004645 0.000001 ( 0.000001 0.000001 0.000001 ) -0.000005 0.000001 0.004639 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066186 0.015243 0.006615 ( 0.000012 0.000012 0.000012 ) -0.016280 0.064853 0.013216 ( 0.000010 0.000010 0.000011 ) -0.003427 -0.014389 0.066491 ( 0.000014 0.000014 0.000014 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000000 ) UB fit with 1403 obs out of 1721 (total:1721,skipped:0) (81.52%) unit cell: 10.3935(18) 10.4069(16) 10.414(2) 90.015(15) 89.936(15) 90.029(13) V = 1126.4(3) unit cell: 10.4046(5) 10.4046(5) 10.4046(5) 90.0 90.0 90.0 V = 1126.37(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= -24.51 ka= -68.11 ph= 119.34 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_1" UB fit with 187 obs out of 220 (total:220,skipped:0) (85.00%) UB - matrix: 0.066500 0.011702 0.008960 ( 0.000032 0.000043 0.000036 ) -0.013689 0.065058 0.013249 ( 0.000030 0.000040 0.000034 ) -0.006052 -0.013931 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000028 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000028 0.004564 0.000048 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000048 0.004603 ( 0.000003 0.000004 0.000005 ) unit cell: 10.406(5) 10.500(6) 10.456(6) 90.60(5) 90.20(4) 89.65(4) V = 1142(1) OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 OTKP changes: 189 1 1 1 Run 1 Omega scan: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) HKL list info: 1312 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004646 -0.000029 0.000015 ( 0.000004 0.000004 0.000003 ) -0.000029 0.004562 0.000049 ( 0.000004 0.000006 0.000004 ) 0.000015 0.000049 0.004603 ( 0.000003 0.000004 0.000005 ) Constraint UB - matrix: 0.066498 0.011703 0.008957 ( 0.000032 0.000043 0.000036 ) -0.013705 0.065046 0.013252 ( 0.000031 0.000042 0.000035 ) -0.006048 -0.013929 0.065931 ( 0.000035 0.000046 0.000039 ) M - matrix: 0.004626 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.004626 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.004626 ( 0.000000 0.000000 0.000002 ) UB fit with 189 obs out of 220 (total:220,skipped:0) (85.91%) unit cell: 10.406(5) 10.502(6) 10.456(6) 90.61(5) 90.19(4) 89.64(4) V = 1143(1) unit cell: 10.4543(19) 10.4543(19) 10.4543(19) 90.0 90.0 90.0 V = 1142.6(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 203 obs out of 220 (total:220,skipped:0) (92.27%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004644 -0.000023 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000023 0.004570 0.000038 ( 0.000003 0.000005 0.000003 ) 0.000007 0.000038 0.004617 ( 0.000003 0.000003 0.000003 ) Constraint UB - matrix: 0.068145 -0.000274 0.000141 ( 0.000028 0.000036 0.000029 ) -0.000059 0.067604 0.000636 ( 0.000031 0.000040 0.000032 ) -0.000037 -0.000066 0.067945 ( 0.000023 0.000029 0.000024 ) M - matrix: 0.004629 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004629 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004629 ( 0.000000 0.000000 0.000001 ) UB fit with 206 obs out of 220 (total:220,skipped:0) (93.64%) unit cell: 10.409(4) 10.492(6) 10.439(4) 90.48(4) 90.09(3) 89.72(4) V = 1140.0(9) unit cell: 10.4466(13) 10.4466(13) 10.4466(13) 90.0 90.0 90.0 V = 1140.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -68.11 ph= 119.34 BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=103, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=79, end=103, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_1_79.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_1_79.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_1_79.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= 24.25 ka= -68.11 ph= -24.52 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_2" UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) UB - matrix: 0.066336 0.014186 0.006779 ( 0.000027 0.000035 0.000035 ) -0.015582 0.064704 0.012861 ( 0.000017 0.000022 0.000023 ) -0.004076 -0.014197 0.066901 ( 0.000019 0.000024 0.000024 ) M - matrix: 0.004660 -0.000009 -0.000023 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000023 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) unit cell: 10.391(4) 10.470(3) 10.361(4) 89.73(3) 89.71(3) 89.88(3) V = 1127.2(7) OTKP changes: 254 1 1 1 OTKP changes: 254 1 1 1 No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) HKL list info: 1303 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004661 -0.000009 -0.000024 ( 0.000004 0.000003 0.000003 ) -0.000009 0.004589 -0.000021 ( 0.000003 0.000003 0.000002 ) -0.000024 -0.000021 0.004687 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: 0.066344 0.014187 0.006783 ( 0.000027 0.000035 0.000035 ) -0.015578 0.064699 0.012866 ( 0.000017 0.000023 0.000023 ) -0.004088 -0.014199 0.066899 ( 0.000018 0.000024 0.000024 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.390(4) 10.471(3) 10.361(4) 89.74(3) 89.71(3) 89.89(3) V = 1127.1(7) unit cell: 10.4069(5) 10.4069(5) 10.4069(5) 90.0 90.0 90.0 V = 1127.10(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004657 -0.000005 -0.000020 ( 0.000003 0.000002 0.000002 ) -0.000005 0.004609 -0.000011 ( 0.000002 0.000003 0.000002 ) -0.000020 -0.000011 0.004676 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: 0.068245 -0.000102 -0.000277 ( 0.000021 0.000027 0.000027 ) 0.000024 0.067891 -0.000164 ( 0.000017 0.000022 0.000022 ) -0.000011 -0.000001 0.068377 ( 0.000015 0.000019 0.000019 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 254 obs out of 254 (total:254,skipped:0) (100.00%) unit cell: 10.393(3) 10.448(3) 10.373(3) 89.86(2) 89.76(3) 89.93(3) V = 1126.4(6) unit cell: 10.4047(5) 10.4047(5) 10.4047(5) 90.0 90.0 90.0 V = 1126.40(10) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -68.11 ph= -24.52 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_2_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_2_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_2_80.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= 24.25 ka= -66.11 ph= -128.46 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_3" UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) UB - matrix: 0.065889 0.015210 0.006808 ( 0.000019 0.000013 0.000019 ) -0.016068 0.064789 0.013228 ( 0.000017 0.000012 0.000017 ) -0.003634 -0.014511 0.066503 ( 0.000022 0.000015 0.000021 ) M - matrix: 0.004613 0.000014 -0.000006 ( 0.000003 0.000001 0.000002 ) 0.000014 0.004640 -0.000004 ( 0.000001 0.000002 0.000002 ) -0.000006 -0.000004 0.004644 ( 0.000002 0.000002 0.000003 ) unit cell: 10.444(3) 10.413(2) 10.408(3) 89.946(19) 89.93(2) 90.171(19) V = 1131.9(5) OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 OTKP changes: 239 1 1 1 No constraint UB - matrix: 0.065942 0.015230 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016127 0.064854 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003636 -0.014463 0.066584 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004622 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004647 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004655 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065942 0.015230 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016127 0.064854 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003636 -0.014463 0.066584 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.434(3) 10.4049(19) 10.396(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.6(5) unit cell: 10.4115(5) 10.4115(5) 10.4115(5) 90.0 90.0 90.0 V = 1128.60(10) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.024) HKL list info: 1275 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.065942 0.015230 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016127 0.064854 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003636 -0.014463 0.066584 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004622 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004647 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004655 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065942 0.015230 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016127 0.064854 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003636 -0.014463 0.066584 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.434(3) 10.4049(19) 10.396(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.6(5) unit cell: 10.4115(5) 10.4115(5) 10.4115(5) 90.0 90.0 90.0 V = 1128.60(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 239 obs out of 239 (total:239,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) ******* No constraint UB - matrix: 0.065942 0.015230 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016127 0.064854 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003636 -0.014463 0.066584 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004622 0.000011 -0.000009 ( 0.000003 0.000001 0.000002 ) 0.000011 0.004647 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000009 -0.000000 0.004655 ( 0.000002 0.000001 0.000003 ) Constraint UB - matrix: 0.065942 0.015230 0.006783 ( 0.000020 0.000014 0.000019 ) -0.016127 0.064854 0.013251 ( 0.000016 0.000011 0.000016 ) -0.003636 -0.014463 0.066584 ( 0.000020 0.000014 0.000019 ) M - matrix: 0.004645 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004645 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004645 ( 0.000000 0.000000 0.000000 ) UB fit with 239 obs out of 239 (total:239,skipped:0) (100.00%) unit cell: 10.434(3) 10.4049(19) 10.396(3) 89.997(18) 89.89(2) 90.136(18) V = 1128.6(5) unit cell: 10.4115(5) 10.4115(5) 10.4115(5) 90.0 90.0 90.0 V = 1128.60(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= -66.11 ph= -128.46 BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=102, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=78, end=102, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_3_78.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_3_78.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_3_78.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= 24.25 ka= 68.89 ph= 0.28 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_4" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: 0.066124 0.015257 0.006585 ( 0.000015 0.000020 0.000017 ) -0.016343 0.064741 0.012922 ( 0.000012 0.000016 0.000013 ) -0.003350 -0.014204 0.066521 ( 0.000011 0.000014 0.000012 ) M - matrix: 0.004651 -0.000002 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000002 0.004626 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.004635 ( 0.000001 0.000001 0.000002 ) unit cell: 10.401(2) 10.429(2) 10.4181(19) 89.903(16) 90.017(17) 89.980(19) V = 1130.0(4) OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 OTKP changes: 222 1 1 1 No constraint UB - matrix: 0.066161 0.015275 0.006524 ( 0.000013 0.000018 0.000015 ) -0.016371 0.064796 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003342 -0.014170 0.066620 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004656 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004633 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066161 0.015275 0.006524 ( 0.000013 0.000018 0.000015 ) -0.016371 0.064796 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003342 -0.014170 0.066620 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.394(2) 10.421(2) 10.4031(18) 89.945(16) 89.960(15) 89.965(18) V = 1126.9(4) unit cell: 10.4062(5) 10.4062(5) 10.4062(5) 90.0 90.0 90.0 V = 1126.89(10) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.024) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066161 0.015275 0.006524 ( 0.000013 0.000018 0.000015 ) -0.016371 0.064796 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003342 -0.014170 0.066620 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004656 -0.000003 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000003 0.004633 -0.000004 ( 0.000001 0.000002 0.000001 ) -0.000003 -0.000004 0.004649 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066161 0.015275 0.006524 ( 0.000013 0.000018 0.000015 ) -0.016371 0.064796 0.012962 ( 0.000012 0.000016 0.000013 ) -0.003342 -0.014170 0.066620 ( 0.000010 0.000013 0.000011 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.394(2) 10.421(2) 10.4031(18) 89.945(16) 89.960(15) 89.965(18) V = 1126.9(4) unit cell: 10.4062(5) 10.4062(5) 10.4062(5) 90.0 90.0 90.0 V = 1126.89(10) 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! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: 0.068223 -0.000038 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068079 -0.000054 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068184 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004654 -0.000003 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.004635 -0.000003 ( 0.000001 0.000002 0.000001 ) -0.000002 -0.000003 0.004649 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068223 -0.000038 -0.000037 ( 0.000011 0.000014 0.000012 ) 0.000001 0.068079 -0.000054 ( 0.000014 0.000018 0.000015 ) 0.000008 0.000010 0.068184 ( 0.000009 0.000012 0.000010 ) M - matrix: 0.004647 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004647 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004647 ( 0.000000 0.000000 0.000000 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 10.3969(16) 10.419(3) 10.4028(15) 89.963(16) 89.976(13) 89.969(17) V = 1126.9(4) unit cell: 10.4061(5) 10.4061(5) 10.4061(5) 90.0 90.0 90.0 V = 1126.85(10) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 68.89 ph= 0.28 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_4_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_4_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_4_80.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= 24.25 ka= 69.89 ph= 92.09 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_5" UB fit with 266 obs out of 271 (total:271,skipped:0) (98.15%) UB - matrix: 0.065977 0.015332 0.006327 ( 0.000017 0.000012 0.000013 ) -0.016376 0.064795 0.013412 ( 0.000019 0.000014 0.000015 ) -0.002889 -0.014585 0.066487 ( 0.000018 0.000014 0.000014 ) M - matrix: 0.004630 -0.000007 0.000006 ( 0.000002 0.000002 0.000002 ) -0.000007 0.004646 -0.000004 ( 0.000002 0.000002 0.000001 ) 0.000006 -0.000004 0.004640 ( 0.000002 0.000001 0.000002 ) unit cell: 10.425(2) 10.406(2) 10.412(2) 89.955(17) 90.071(19) 89.909(19) V = 1129.5(4) OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 OTKP changes: 270 1 1 1 No constraint UB - matrix: 0.066057 0.015391 0.006336 ( 0.000016 0.000012 0.000013 ) -0.016401 0.064855 0.013376 ( 0.000018 0.000014 0.000014 ) -0.002879 -0.014634 0.066572 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004641 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004657 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004651 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066057 0.015391 0.006336 ( 0.000016 0.000012 0.000013 ) -0.016401 0.064855 0.013376 ( 0.000018 0.000014 0.000014 ) -0.002879 -0.014634 0.066572 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.412(2) 10.394(2) 10.4007(18) 89.887(15) 90.093(17) 89.940(18) V = 1125.5(4) unit cell: 10.4021(5) 10.4021(5) 10.4021(5) 90.0 90.0 90.0 V = 1125.54(10) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.024) HKL list info: 1298 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066057 0.015391 0.006336 ( 0.000016 0.000012 0.000013 ) -0.016401 0.064855 0.013376 ( 0.000018 0.000014 0.000014 ) -0.002879 -0.014634 0.066572 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004641 -0.000005 0.000008 ( 0.000002 0.000001 0.000001 ) -0.000005 0.004657 -0.000009 ( 0.000001 0.000002 0.000001 ) 0.000008 -0.000009 0.004651 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.066057 0.015391 0.006336 ( 0.000016 0.000012 0.000013 ) -0.016401 0.064855 0.013376 ( 0.000018 0.000014 0.000014 ) -0.002879 -0.014634 0.066572 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.412(2) 10.394(2) 10.4007(18) 89.887(15) 90.093(17) 89.940(18) V = 1125.5(4) unit cell: 10.4021(5) 10.4021(5) 10.4021(5) 90.0 90.0 90.0 V = 1125.54(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: 0.068128 -0.000095 0.000072 ( 0.000017 0.000013 0.000014 ) 0.000060 0.068213 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068190 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004641 -0.000002 0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.004653 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000006 0.004650 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.068128 -0.000095 0.000072 ( 0.000017 0.000013 0.000014 ) 0.000060 0.068213 -0.000092 ( 0.000014 0.000010 0.000011 ) -0.000019 0.000009 0.068190 ( 0.000015 0.000011 0.000012 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000000 ) UB fit with 270 obs out of 271 (total:271,skipped:0) (99.63%) unit cell: 10.411(3) 10.3983(16) 10.4018(18) 89.930(13) 90.044(17) 89.970(16) V = 1126.1(4) unit cell: 10.4038(5) 10.4038(5) 10.4038(5) 90.0 90.0 90.0 V = 1126.09(10) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= 24.25 ka= 69.89 ph= 92.09 BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=104, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=80, end=104, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_5_80.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_5_80.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_5_80.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= -24.51 ka= -38.11 ph= -180.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-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\xs2212a\tmp\xs2212a_proffitpeak_6" UB fit with 182 obs out of 190 (total:190,skipped:0) (95.79%) UB - matrix: 0.066063 0.015588 0.006255 ( 0.000020 0.000017 0.000019 ) -0.016421 0.064837 0.013096 ( 0.000027 0.000023 0.000026 ) -0.002974 -0.014212 0.066498 ( 0.000033 0.000028 0.000032 ) M - matrix: 0.004643 0.000007 0.000000 ( 0.000003 0.000002 0.000003 ) 0.000007 0.004649 0.000001 ( 0.000002 0.000003 0.000003 ) 0.000000 0.000001 0.004633 ( 0.000003 0.000003 0.000004 ) unit cell: 10.410(3) 10.403(4) 10.421(5) 90.02(3) 90.01(3) 90.09(3) V = 1128.5(7) OTKP changes: 190 1 1 1 OTKP changes: 190 1 1 1 No constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004638 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.415(3) 10.421(3) 10.405(2) 89.85(2) 90.17(2) 90.10(2) V = 1129.2(5) unit cell: 10.4134(7) 10.4134(7) 10.4134(7) 90.0 90.0 90.0 V = 1129.23(13) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) HKL list info: 1267 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004638 0.000008 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000008 0.004633 -0.000012 ( 0.000002 0.000003 0.000002 ) 0.000013 -0.000012 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.066033 0.015585 0.006344 ( 0.000019 0.000016 0.000018 ) -0.016420 0.064683 0.013080 ( 0.000022 0.000019 0.000022 ) -0.002864 -0.014366 0.066603 ( 0.000014 0.000012 0.000014 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.415(3) 10.421(3) 10.405(2) 89.85(2) 90.17(2) 90.10(2) V = 1129.2(5) unit cell: 10.4134(7) 10.4134(7) 10.4134(7) 90.0 90.0 90.0 V = 1129.23(13) 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! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: 0.068131 0.000083 0.000194 ( 0.000020 0.000016 0.000019 ) -0.000013 0.068074 -0.000160 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068166 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000005 0.000013 ( 0.000003 0.000002 0.000002 ) 0.000005 0.004634 -0.000011 ( 0.000002 0.000002 0.000002 ) 0.000013 -0.000011 0.004647 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: 0.068131 0.000083 0.000194 ( 0.000020 0.000016 0.000019 ) -0.000013 0.068074 -0.000160 ( 0.000021 0.000017 0.000020 ) -0.000002 0.000001 0.068166 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.004642 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004642 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004642 ( 0.000000 0.000000 0.000001 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 10.411(3) 10.420(3) 10.4055(18) 89.867(19) 90.161(19) 90.06(2) V = 1128.7(5) unit cell: 10.4120(7) 10.4120(7) 10.4120(7) 90.0 90.0 90.0 V = 1128.75(12) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= -38.11 ph= -180.00 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\xs2212a\tmp\xs2212a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_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\xs2212a\tmp\xs2212a_back_6_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_6_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_6_75.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= -24.51 ka= 56.89 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\xs2212a\tmp\xs2212a_proffitpeak_7" UB fit with 91 obs out of 101 (total:101,skipped:0) (90.10%) UB - matrix: 0.066127 0.015391 0.006100 ( 0.000089 0.000045 0.000045 ) -0.016533 0.064614 0.013419 ( 0.000046 0.000024 0.000023 ) -0.002820 -0.014456 0.066486 ( 0.000081 0.000041 0.000041 ) M - matrix: 0.004654 -0.000010 -0.000006 ( 0.000012 0.000005 0.000006 ) -0.000010 0.004621 -0.000000 ( 0.000005 0.000004 0.000003 ) -0.000006 -0.000000 0.004638 ( 0.000006 0.000003 0.000006 ) unit cell: 10.397(13) 10.435(5) 10.415(6) 90.00(4) 89.93(7) 89.88(6) V = 1130(2) OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 OTKP changes: 101 1 1 1 No constraint UB - matrix: 0.066212 0.015412 0.005951 ( 0.000054 0.000029 0.000028 ) -0.016508 0.064728 0.013537 ( 0.000030 0.000016 0.000016 ) -0.002356 -0.014565 0.066557 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004662 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004639 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000001 0.004649 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066212 0.015412 0.005951 ( 0.000054 0.000029 0.000028 ) -0.016508 0.064728 0.013537 ( 0.000030 0.000016 0.000016 ) -0.002356 -0.014565 0.066557 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.388(8) 10.414(3) 10.403(3) 89.98(2) 90.17(3) 89.83(4) V = 1125.4(10) unit cell: 10.4017(9) 10.4017(9) 10.4017(9) 90.0 90.0 90.0 V = 1125.42(18) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.024) HKL list info: 674 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066212 0.015412 0.005951 ( 0.000054 0.000029 0.000028 ) -0.016508 0.064728 0.013537 ( 0.000030 0.000016 0.000016 ) -0.002356 -0.014565 0.066557 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004662 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004639 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000001 0.004649 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.066212 0.015412 0.005951 ( 0.000054 0.000029 0.000028 ) -0.016508 0.064728 0.013537 ( 0.000030 0.000016 0.000016 ) -0.002356 -0.014565 0.066557 ( 0.000032 0.000017 0.000017 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.388(8) 10.414(3) 10.403(3) 89.98(2) 90.17(3) 89.83(4) V = 1125.4(10) unit cell: 10.4017(9) 10.4017(9) 10.4017(9) 90.0 90.0 90.0 V = 1125.42(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 7) ******* No constraint UB - matrix: 0.068286 -0.000191 0.000206 ( 0.000053 0.000028 0.000028 ) -0.000007 0.068113 -0.000019 ( 0.000031 0.000017 0.000016 ) 0.000000 -0.000002 0.068179 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004663 -0.000014 0.000014 ( 0.000007 0.000003 0.000003 ) -0.000014 0.004639 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000014 -0.000001 0.004648 ( 0.000003 0.000002 0.000002 ) Constraint UB - matrix: 0.068286 -0.000191 0.000206 ( 0.000053 0.000028 0.000028 ) -0.000007 0.068113 -0.000019 ( 0.000031 0.000017 0.000016 ) 0.000000 -0.000002 0.068179 ( 0.000033 0.000018 0.000017 ) M - matrix: 0.004646 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004646 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004646 ( 0.000000 0.000000 0.000001 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 10.387(8) 10.414(2) 10.404(3) 89.98(2) 90.17(4) 89.83(3) V = 1125.3(10) unit cell: 10.4014(9) 10.4014(9) 10.4014(9) 90.0 90.0 90.0 V = 1125.33(18) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 56.89 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=47, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=23, end=47, BACKGROUND INFO: Using background file D:\Data\xs2212a\tmp\xs2212a_back_7_23.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_7_23.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_7_23.rpb *** 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= -24.51 ka= 37.89 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\xs2212a\tmp\xs2212a_proffitpeak_8" UB fit with 188 obs out of 224 (total:224,skipped:0) (83.93%) UB - matrix: 0.066011 0.015526 0.005995 ( 0.000038 0.000022 0.000028 ) -0.016682 0.064707 0.013481 ( 0.000025 0.000015 0.000018 ) -0.002628 -0.014357 0.066560 ( 0.000044 0.000026 0.000032 ) M - matrix: 0.004643 -0.000017 -0.000004 ( 0.000005 0.000002 0.000003 ) -0.000017 0.004634 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000004 0.000010 0.004648 ( 0.000003 0.000002 0.000004 ) unit cell: 10.410(5) 10.419(3) 10.404(5) 90.12(3) 89.95(4) 89.79(3) V = 1128.5(8) OTKP changes: 224 1 1 1 OTKP changes: 224 1 1 1 OTKP changes: 224 1 1 1 No constraint UB - matrix: 0.066018 0.015598 0.005897 ( 0.000022 0.000015 0.000019 ) -0.016635 0.064735 0.013569 ( 0.000020 0.000013 0.000017 ) -0.002247 -0.014622 0.066614 ( 0.000015 0.000010 0.000013 ) M - matrix: 0.004640 -0.000014 0.000014 ( 0.000003 0.000002 0.000002 ) -0.000014 0.004648 -0.000004 ( 0.000002 0.000002 0.000001 ) 0.000014 -0.000004 0.004656 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.066018 0.015598 0.005897 ( 0.000022 0.000015 0.000019 ) -0.016635 0.064735 0.013569 ( 0.000020 0.000013 0.000017 ) -0.002247 -0.014622 0.066614 ( 0.000015 0.000010 0.000013 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000001 ) UB fit with 224 obs out of 224 (total:224,skipped:0) (100.00%) unit cell: 10.413(3) 10.404(2) 10.395(2) 89.955(17) 90.17(2) 89.82(2) V = 1126.1(5) unit cell: 10.4039(6) 10.4039(6) 10.4039(6) 90.0 90.0 90.0 V = 1126.13(12) Run 8 Omega scan: (-49.000 - 50.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.024) HKL list info: 1244 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: 0.066018 0.015598 0.005897 ( 0.000022 0.000015 0.000019 ) -0.016635 0.064735 0.013569 ( 0.000020 0.000013 0.000017 ) -0.002247 -0.014622 0.066614 ( 0.000015 0.000010 0.000013 ) M - matrix: 0.004640 -0.000014 0.000014 ( 0.000003 0.000002 0.000002 ) -0.000014 0.004648 -0.000004 ( 0.000002 0.000002 0.000001 ) 0.000014 -0.000004 0.004656 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.066018 0.015598 0.005897 ( 0.000022 0.000015 0.000019 ) -0.016635 0.064735 0.013569 ( 0.000020 0.000013 0.000017 ) -0.002247 -0.014622 0.066614 ( 0.000015 0.000010 0.000013 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000001 ) UB fit with 224 obs out of 224 (total:224,skipped:0) (100.00%) unit cell: 10.413(3) 10.404(2) 10.395(2) 89.955(17) 90.17(2) 89.82(2) V = 1126.1(5) unit cell: 10.4039(6) 10.4039(6) 10.4039(6) 90.0 90.0 90.0 V = 1126.13(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 224 obs out of 224 (total:224,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: 0.068119 -0.000184 0.000177 ( 0.000023 0.000015 0.000020 ) 0.000010 0.068168 -0.000026 ( 0.000015 0.000010 0.000013 ) -0.000022 -0.000007 0.068225 ( 0.000015 0.000010 0.000013 ) M - matrix: 0.004640 -0.000012 0.000011 ( 0.000003 0.000001 0.000002 ) -0.000012 0.004647 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000011 -0.000002 0.004655 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: 0.068119 -0.000184 0.000177 ( 0.000023 0.000015 0.000020 ) 0.000010 0.068168 -0.000026 ( 0.000015 0.000010 0.000013 ) -0.000022 -0.000007 0.068225 ( 0.000015 0.000010 0.000013 ) M - matrix: 0.004648 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.004648 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.004648 ( 0.000000 0.000000 0.000001 ) UB fit with 224 obs out of 224 (total:224,skipped:0) (100.00%) unit cell: 10.413(4) 10.4051(16) 10.397(2) 89.973(14) 90.13(2) 89.854(18) V = 1126.4(5) unit cell: 10.4047(6) 10.4047(6) 10.4047(6) 90.0 90.0 90.0 V = 1126.41(12) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs2212a\tmp\xs2212a_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= -24.51 ka= 37.89 ph= 120.00 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\xs2212a\tmp\xs2212a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_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\xs2212a\tmp\xs2212a_back_8_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs2212a\tmp\xs2212a_backsig_8_75.img BACKGROUND INFO: Using background info file D:\Data\xs2212a\tmp\xs2212a_back_8_75.rpb Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_1" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_2" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_3" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_4" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_5" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_6" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_7" Reading tabbin file: "D:\Data\xs2212a\tmp\xs2212a_proffitpeak_8" PROFFIT INFO: Final refinement of B matrix and unit cell No constraint UB - matrix: 0.068158 -0.000019 -0.000009 ( 0.000008 0.000008 0.000008 ) -0.000006 0.068110 0.000004 ( 0.000008 0.000008 0.000008 ) 0.000022 -0.000010 0.068186 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004645 -0.000002 0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 0.004639 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000001 -0.000000 0.004649 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.068158 -0.000019 -0.000009 ( 0.000008 0.000008 0.000008 ) -0.000006 0.068110 0.000004 ( 0.000008 0.000008 0.000008 ) 0.000022 -0.000010 0.068186 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) UB fit with 1698 obs out of 1721 (total:1721,skipped:0) (98.66%) unit cell: 10.4067(13) 10.4140(12) 10.4024(9) 89.994(8) 90.011(9) 89.979(10) V = 1127.4(2) unit cell: 10.4077(3) 10.4077(3) 10.4077(3) 90.0 90.0 90.0 V = 1127.36(5) Writing tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak" Discarded reflections: 229 reflections under beam stop or inside a detector rejection region Merging .rrpprof files... Adding file D:\Data\xs2212a\tmp\xs2212a_1.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_2.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_3.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_4.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_5.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_6.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_7.rrpprof Adding file D:\Data\xs2212a\tmp\xs2212a_8.rrpprof 7540 reflections saved to the file D:\Data\xs2212a\xs2212a.rrpprof PROFFITMAIN - Finished at Wed Aug 21 15:26:18 2019 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs2212a\xs2212a.rrpprof OUTPUT: D:\Data\xs2212a\xs2212a 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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.024) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.024) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.024) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.024) Run 8 Omega scan: (-49.000 - 50.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.024) PROFFIT INFO: signal sum: min=-784.0000 max=10593745.0000 PROFFIT INFO: signal sum lp corr: min=-736.9381 max=1264135.7702 PROFFIT INFO: background sum: min=-93.0000 max=8245.0000 PROFFIT INFO: background sum sig2: min=440.0000 max=5762.0000 PROFFIT INFO: num of signal pixels: min=41 max=516 PROFFIT INFO: Inet: min=-1179.1011 max=2022617.2500 PROFFIT INFO: sig(Inet): min=52.1889 max=30734.7832 PROFFIT INFO: Inet/sig(Inet): min=-2.12 max=274.23 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 659 2537 3886 4658 5027 5855 6362 6661 7134 7457 7540 Percent 8.7 33.6 51.5 61.8 66.7 77.7 84.4 88.3 94.6 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 7540 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 7540 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2022617- 133444 754 424497.59 79.01 100.00 133172- 4204 754 30192.15 19.62 100.00 4203- 2173 754 2977.95 7.18 97.75 2171- 1276 754 1655.23 3.98 53.18 1276- 848 754 1046.16 2.40 17.11 848- 562 754 696.50 1.73 8.36 562- 353 754 453.25 1.26 5.04 353- 162 754 254.62 0.75 0.80 162- 20 754 86.32 0.31 0.00 20- -1179 754 -139.32 -0.27 0.00 ------------------------------------------------------------------------------------ 2022617- -1179 7540 46172.05 11.60 38.22 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 754 109379.99 15.57 67.51 1.64- 1.26 754 89844.52 21.46 57.29 1.26- 1.06 754 80034.86 22.70 71.49 1.06- 0.96 754 40449.55 11.41 30.24 0.96- 0.88 754 27614.86 9.60 48.14 0.88- 0.80 754 42710.95 11.98 33.95 0.80- 0.75 754 21986.52 6.60 21.22 0.75- 0.71 754 19936.00 6.51 16.18 0.71- 0.67 754 26011.71 8.28 29.58 0.67- 0.62 754 3751.50 1.84 6.63 ------------------------------------------------------------------------------------ 6.00- 0.62 7540 46172.05 11.60 38.22 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 15:26:19 2019 Sorting 7540 observations 54 unique observations with > 7.00 F2/sig(F2) 7540 observations in 8 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 8 0 98 760 Total number of frames 760 Maximum number of 54 frame scales suggested for reliable scaling Glued frame scales: 15 frame = 1 scale 7540 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 3 46 8 0 6 53 Total number of frames 53 1832 observations > 7.00 F2/sig(F2) 1832 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 3 46 8 0 6 53 Total number of frames 53 Removing 'redundancy=1' reflections Average redundancy: 24.4 (Out of 1832 removed 1 = 1831, unique = 75) 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 1831 observations in 8 runs Run # start # end # total # 1 0 6 7 2 0 6 14 3 0 6 21 4 0 6 28 5 0 6 35 6 0 6 42 7 0 3 46 8 0 6 53 Total number of frames 53 75 unique data precomputed (should be 75) 75 unique data with 1831 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 24.4 (Out of 1831 removed 0 = 1831, unique = 75) 75 unique data precomputed (should be 75) 75 unique data with 1831 observations RMS deviation of equivalent data = 0.31869 Rint = 0.25950 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.25269, wR= 0.34345 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13431, wR= 0.18219, Acormin=0.466, Acormax=1.454, Acor_av=0.975 F test: Probability=1.000, F= 3.530 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13433, wR= 0.17854, Acormin=0.453, Acormax=1.501, Acor_av=0.969 F test: Probability=0.000, F= 0.998 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12523, wR= 0.17275, Acormin=0.555, Acormax=1.552, Acor_av=0.983 F test: Probability=0.998, F= 1.144 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12537, wR= 0.16828, Acormin=0.519, Acormax=1.563, Acor_av=0.979 F test: Probability=0.000, F= 0.996 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10649, wR= 0.14939, Acormin=0.567, Acormax=1.828, Acor_av=1.011 F test: Probability=1.000, F= 1.375 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11958, wR= 0.16604, Acormin=0.453, Acormax=1.645, Acor_av=0.968 F test: Probability=0.000, F= 0.792 Trying model 7 (ne=6, no=1)... Results: Rint= 0.11906, wR= 0.16276, Acormin=0.449, Acormax=1.630, Acor_av=0.966 F test: Probability=0.000, F= 0.797 Trying model 8 (ne=6, no=3)... Results: Rint= 0.10205, wR= 0.14571, Acormin=0.494, Acormax=1.839, Acor_av=0.996 F test: Probability=0.946, F= 1.081 Trying model 9 (ne=6, no=5)... Results: Rint= 0.15723, wR= 0.19894, Acormin=0.115, Acormax=1.225, Acor_av=0.534 F test: Probability=0.000, F= 0.452 Final absorption model (ne=4, no=3): Rint= 0.10649, Acormin=0.567, Acormax=1.828, Acor_av=1.011 Combined refinement in use Rint: 0.26134 There are 53 active scales (one needs to be fixed) Refinement control: frame scale #32 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 76 pars with 2926 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31869 Using Levenberg-Marquardt: 0.00010 New wR= 0.10467 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25950 with corrections 0.08058 Rint for all data: 0.26134 with corrections 0.08326 4 observations identified as outliers and rejected Cycle 2 wR= 0.09538 Using Levenberg-Marquardt: 0.00001 New wR= 0.08031 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25983 with corrections 0.05912 Rint for all data: 0.26134 with corrections 0.06460 1 observations identified as outliers and rejected Cycle 3 wR= 0.07740 Using Levenberg-Marquardt: 0.00000 New wR= 0.07464 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25861 with corrections 0.05434 Rint for all data: 0.26134 with corrections 0.06024 2 observations identified as outliers and rejected Cycle 4 wR= 0.07043 Using Levenberg-Marquardt: 0.00000 New wR= 0.06937 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25802 with corrections 0.05112 Rint for all data: 0.26134 with corrections 0.05746 2 observations identified as outliers and rejected Cycle 5 wR= 0.06424 Using Levenberg-Marquardt: 0.00000 New wR= 0.06298 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25676 with corrections 0.04813 Rint for all data: 0.26134 with corrections 0.05537 1 observations identified as outliers and rejected Final wR= 0.06298 Final frame scales: Min= 0.7545 Max= 1.2690 Final absorption correction factors: Amin= 0.3699 Amax= 1.5738 PROFFIT INFO: Inet (after scale3 abspack): min=-1169.0659 max=1306399.6250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=39.5771 max=24544.2461 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/104 7540 reflections read from tmp file 279 reflections are rejected (278 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 1 5 2 2 2 6 5 215 Initial Chi^2= 0.51368 Cycle 1, Chi^2= 1.00829 Current error model SIG(F2)^2 = 56.14*I_RAW + 13.01*I_BACK+(0.03732*)^2 Cycle 2, Chi^2= 1.01072 Current error model SIG(F2)^2 = 70.18*I_RAW + 9.55*I_BACK+(0.02954*)^2 Cycle 3, Chi^2= 1.00649 Current error model SIG(F2)^2 = 76.70*I_RAW + 8.18*I_BACK+(0.02673*)^2 Cycle 4, Chi^2= 1.00266 Current error model SIG(F2)^2 = 79.24*I_RAW + 7.71*I_BACK+(0.02590*)^2 Cycle 5, Chi^2= 1.00087 Current error model SIG(F2)^2 = 80.08*I_RAW + 7.56*I_BACK+(0.02567*)^2 Cycle 6, Chi^2= 1.00026 Current error model SIG(F2)^2 = 80.33*I_RAW + 7.52*I_BACK+(0.02561*)^2 Cycle 7, Chi^2= 1.00007 Current error model SIG(F2)^2 = 80.40*I_RAW + 7.50*I_BACK+(0.02560*)^2 Final Chi^2= 1.00007 Final error model SIG(F2)^2 = 80.40*I_RAW + 7.50*I_BACK+(0.02560*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1306400- 121088 754 389520.14 31.69 100.00 121046- 3593 754 30322.57 13.58 100.00 3592- 2070 754 2773.64 6.39 99.47 2067- 1198 754 1553.10 4.07 71.88 1197- 797 754 979.40 2.90 32.10 797- 537 754 664.04 2.45 16.98 536- 339 754 432.75 1.99 8.89 338- 158 754 250.47 1.48 3.85 158- 20 754 84.70 0.74 0.40 20- -1169 754 -139.84 -0.56 0.00 ------------------------------------------------------------------------------------ 1306400- -1169 7540 42644.10 6.47 43.36 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 754 104890.43 10.41 71.75 1.64- 1.26 754 82506.50 9.57 61.01 1.26- 1.06 754 72176.94 9.81 77.06 1.06- 0.96 754 37340.52 5.59 33.02 0.96- 0.88 754 25082.26 6.05 57.43 0.88- 0.80 754 39533.94 6.70 42.04 0.80- 0.75 754 19817.54 4.37 24.93 0.75- 0.71 754 18128.08 4.74 22.15 0.71- 0.67 754 23443.48 5.69 34.35 0.67- 0.62 754 3521.28 1.78 9.81 ------------------------------------------------------------------------------------ 6.00- 0.62 7540 42644.10 6.47 43.36 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 754 104890.43 10.41 71.75 6.00- 1.26 1508 93698.47 9.99 66.38 6.00- 1.06 2262 86524.62 9.93 69.94 6.00- 0.96 3016 74228.60 8.85 60.71 6.00- 0.88 3770 64399.33 8.29 60.05 6.00- 0.80 4524 60255.10 8.02 57.05 6.00- 0.75 5278 54478.30 7.50 52.46 6.00- 0.71 6032 49934.53 7.16 48.67 6.00- 0.67 6786 46991.08 6.99 47.08 6.00- 0.62 7540 42644.10 6.47 43.36 ------------------------------------------------------------------------------------ 6.00- 0.62 7540 42644.10 6.47 43.36 Scale applied to data: s=0.765462 (maximum obs:1306399.625,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.055; Rsigma 0.037: data 7540 -> merged 241 With outlier rejection... Rint 0.050; Rsigma 0.037: data 7521 -> merged 241 Rejected total: 19, method kkm 11, method Blessing 8 Completeness direct cell (a, b, c) = (10.408, 10.408, 10.408), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.621979, 6.008889 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 10.41 - 1.59 21 21 40.24 100.00 845 1.57 - 1.20 21 21 42.24 100.00 887 1.19 - 1.02 21 21 40.24 100.00 845 1.02 - 0.91 21 21 38.71 100.00 813 0.91 - 0.84 21 21 34.38 100.00 722 0.84 - 0.78 21 21 33.67 100.00 707 0.78 - 0.74 21 21 31.71 100.00 666 0.74 - 0.71 21 21 27.00 100.00 567 0.71 - 0.68 21 21 29.52 100.00 620 0.68 - 0.65 23 23 25.30 100.00 582 --------------------------------------------------------------- 10.41 - 0.65 212 212 34.22 100.00 7254 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 15:26:19 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.406726 10.413986 10.402395 89.9944 90.0108 89.9792 7521 Reflections read from file xs2212a.hkl 7521 Reflections used for space-group determination (up to diffraction limit of 0.62A); mean (I/sigma) = 6.45 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3772 0 4989 4989 7521 N (int>3sigma) = 0 0 0 0 1747 0 2278 2248 3256 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.5 31.8 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.6 6.5 6.5 Lattice type: F chosen Volume: 1127.36 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 0.5000 Unitcell: 7.356 7.358 7.359 119.99 119.96 90.02 Niggli form: a.a = 54.117 b.b = 54.138 c.c = 54.160 b.c = -27.065 a.c = -27.035 a.b = -0.023 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.097 CUBIC F-lattice R(int) = 0.050 [ 7280] Vol = 1127.4 Cell: 10.414 10.407 10.402 89.99 90.01 89.98 Volume: 1127.36 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.052 TETRAGONAL I-lattice R(int) = 0.050 [ 6882] Vol = 563.7 Cell: 7.360 7.363 10.402 90.00 89.99 89.96 Volume: 563.68 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.039 TETRAGONAL I-lattice R(int) = 0.050 [ 6879] Vol = 563.7 Cell: 7.356 7.358 10.414 90.01 89.98 90.02 Volume: 563.68 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.049 TETRAGONAL I-lattice R(int) = 0.050 [ 6882] Vol = 563.7 Cell: 7.363 7.360 10.402 90.01 90.00 90.04 Volume: 563.68 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.041 ORTHORHOMBIC F-lattice R(int) = 0.049 [ 6828] Vol = 1127.4 Cell: 10.402 10.407 10.414 89.98 90.01 89.99 Volume: 1127.36 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.055 ORTHORHOMBIC I-lattice R(int) = 0.049 [ 6807] Vol = 563.7 Cell: 10.402 7.363 7.360 89.96 89.99 90.00 Volume: 563.68 Matrix: 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.033 ORTHORHOMBIC I-lattice R(int) = 0.049 [ 6808] Vol = 563.7 Cell: 7.356 7.358 10.414 89.99 90.02 90.02 Volume: 563.68 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.023 MONOCLINIC I-lattice R(int) = 0.047 [ 6270] Vol = 563.7 Cell: 7.360 10.402 7.363 90.00 90.04 90.01 Volume: 563.68 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.032 MONOCLINIC I-lattice R(int) = 0.048 [ 6269] Vol = 563.7 Cell: 7.359 10.407 7.360 90.01 90.06 89.98 Volume: 563.68 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.021 MONOCLINIC I-lattice R(int) = 0.047 [ 6270] Vol = 563.7 Cell: 7.363 10.402 7.360 90.01 90.04 90.00 Volume: 563.68 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.023 MONOCLINIC I-lattice R(int) = 0.047 [ 6248] Vol = 563.7 Cell: 7.356 7.358 10.414 90.01 90.02 89.98 Volume: 563.68 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.014 MONOCLINIC I-lattice R(int) = 0.047 [ 6269] Vol = 563.7 Cell: 7.356 10.414 7.358 90.01 90.02 89.98 Volume: 563.68 Matrix: 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.025 MONOCLINIC I-lattice R(int) = 0.047 [ 6269] Vol = 563.7 Cell: 7.356 10.414 7.358 89.99 90.02 90.02 Volume: 563.68 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) = 0.044 [ 5195] Vol = 281.8 Cell: 7.356 7.358 7.359 119.99 119.96 90.02 Volume: 281.84 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 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 3772 0 4989 4989 7521 N (int>3sigma) = 0 0 0 0 1747 0 2278 2248 3256 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.5 31.8 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.6 6.5 6.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.676 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 57 57 560 1473 N I>3s 2 2 3 803 0.0 0.0 -0.0 1.9 0.8 0.8 0.2 5.1 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 0.050 6748 Fd-3m 1 1 227 C N N N N 37 2284 0.050 6814 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.413986 10.406726 10.402395 89.9892 90.0056 89.9792 ZERR 5.00 0.001186 0.001279 0.000906 0.0086 0.0083 0.0096 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1170006- 132340 749 740 26 28.5 391214.85 31.78 0.046 0.061 112586- 3305 853 849 26 32.7 27951.72 12.77 0.061 0.077 3130- 1454 1078 1076 26 41.4 2294.17 5.79 0.126 0.179 1403- 885 958 958 26 36.8 1094.86 2.91 0.227 0.296 871- 544 864 864 26 33.2 676.58 2.40 0.304 0.408 541- 326 920 919 26 35.3 417.65 1.86 0.412 0.555 320- 147 730 729 26 28.0 245.09 1.36 0.557 0.976 143- 22 739 739 26 28.4 73.01 0.56 0.878 2.552 21- -225 649 647 33 19.6 -28.42 -0.07 0.987 4.322 ------------------------------------------------------------------------------------------- 1170006- -225 7540 7521 241 31.2 42272.31 6.45 0.050 0.067 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-1.44 1087 1083 26 41.7 119721.53 11.63 0.049 0.063 0.028 1.39-1.09 1148 1146 26 44.1 45995.74 7.68 0.045 0.058 0.033 1.06-0.94 966 963 26 37.0 39936.67 5.86 0.042 0.058 0.035 0.92-0.84 919 918 26 35.3 43127.01 7.75 0.050 0.068 0.040 0.84-0.78 894 892 26 34.3 24847.24 5.15 0.054 0.071 0.046 0.78-0.73 759 757 26 29.1 8867.49 3.22 0.078 0.093 0.073 0.73-0.69 801 800 27 29.6 20058.20 4.91 0.065 0.081 0.058 0.68-0.66 665 663 26 25.5 15522.34 4.10 0.072 0.101 0.065 0.66-0.62 301 299 32 9.3 7680.96 2.37 0.082 0.089 0.086 ------------------------------------------------------------------------------------------------------ inf-0.62 7540 7521 241 31.2 42272.31 6.45 0.050 0.067 0.037 inf-0.65 7269 7252 211 34.4 43590.72 6.61 0.050 0.066 0.036 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-1.44 1083 26 26 100.0 41.7 119721.53 75.91 0.049 0.005 1.39-1.09 1146 26 26 100.0 44.1 45995.74 47.01 0.045 0.006 1.06-0.94 963 26 26 100.0 37.0 39936.67 36.76 0.042 0.006 0.92-0.84 918 26 26 100.0 35.3 43127.01 45.63 0.050 0.007 0.84-0.78 892 26 26 100.0 34.3 24847.24 28.74 0.054 0.008 0.78-0.73 757 26 26 100.0 29.1 8867.49 17.56 0.078 0.014 0.73-0.69 800 27 27 100.0 29.6 20058.20 25.66 0.065 0.011 0.68-0.66 663 26 26 100.0 25.5 15522.34 22.50 0.072 0.013 0.66-0.62 299 33 32 97.0 9.3 7680.96 6.82 0.082 0.032 -------------------------------------------------------------------------------------------- inf-0.62 7521 242 241 99.6 31.2 42272.31 38.53 0.050 0.008 inf-0.65 7252 211 211 100.0 34.4 43590.72 39.72 0.050 0.007 Reading tabbin file: "D:\Data\xs2212a\xs2212a_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: 0.066104 0.015183 0.006666 ( 0.000008 0.000008 0.000008 ) -0.016259 0.064815 0.013213 ( 0.000008 0.000008 0.000008 ) -0.003378 -0.014397 0.066561 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004646 -0.000002 0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 0.004639 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 -0.000001 0.004649 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.066104 0.015183 0.006666 ( 0.000008 0.000008 0.000008 ) -0.016259 0.064815 0.013213 ( 0.000008 0.000008 0.000008 ) -0.003378 -0.014397 0.066561 ( 0.000006 0.000006 0.000006 ) M - matrix: 0.004644 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.004644 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.004644 ( 0.000000 0.000000 0.000000 ) unit cell: 10.4067(13) 10.4142(12) 10.4024(9) 89.992(8) 90.012(8) 89.980(10) V = 1127.4(2) unit cell: 10.4078(3) 10.4078(3) 10.4078(3) 90.0 90.0 90.0 V = 1127.39(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: (-97.000 - 6.000,103 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-68.000,ph=119.338 (rot geo dd=53.134) Run 2 Omega scan: (-49.000 - 55.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-68.000,ph=-24.523 (rot geo dd=53.001) Run 3 Omega scan: (-48.000 - 54.000,102 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=-66.000,ph=-128.461 (rot geo dd=53.024) Run 4 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=69.000,ph=0.280 (rot geo dd=53.024) Run 5 Omega scan: (-6.000 - 98.000,104 frames, 7.500 sec, 1.000 deg) at th=24.461, ka=70.000,ph=92.086 (rot geo dd=53.024) Run 6 Omega scan: (-99.000 - 0.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=-38.000,ph=-180.000 (rot geo dd=53.042) Run 7 Omega scan: (-52.000 - -5.000,47 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=57.000,ph=150.000 (rot geo dd=53.024) Run 8 Omega scan: (-49.000 - 50.000,99 frames, 7.500 sec, 1.000 deg) at th=-24.304, ka=38.000,ph=120.000 (rot geo dd=53.024) PROFFIT INFO: signal sum: min=-784.0000 max=10593745.0000 PROFFIT INFO: signal sum lp corr: min=-736.9381 max=1264135.7702 PROFFIT INFO: background sum: min=-93.0000 max=8245.0000 PROFFIT INFO: background sum sig2: min=440.0000 max=5762.0000 PROFFIT INFO: num of signal pixels: min=41 max=516 PROFFIT INFO: Inet: min=-1179.1011 max=2022617.2500 PROFFIT INFO: sig(Inet): min=52.1889 max=30734.7832 PROFFIT INFO: Inet/sig(Inet): min=-2.12 max=274.23 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 1318 5074 7772 9316 10054 11710 12724 13322 14268 14914 15080 Percent 8.7 33.6 51.5 61.8 66.7 77.7 84.4 88.3 94.6 98.9 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 7540 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 7540 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2022617- 133444 754 424497.59 79.01 100.00 133172- 4204 754 30192.15 19.62 100.00 4203- 2173 754 2977.95 7.18 97.75 2171- 1276 754 1655.23 3.98 53.18 1276- 848 754 1046.16 2.40 17.11 848- 562 754 696.50 1.73 8.36 562- 353 754 453.25 1.26 5.04 353- 162 754 254.62 0.75 0.80 162- 20 754 86.32 0.31 0.00 20- -1179 754 -139.32 -0.27 0.00 ------------------------------------------------------------------------------------ 2022617- -1179 7540 46172.05 11.60 38.22 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 754 109379.99 15.57 67.51 1.64- 1.26 754 89844.52 21.46 57.29 1.26- 1.06 754 80034.86 22.70 71.49 1.06- 0.96 754 40449.55 11.41 30.24 0.96- 0.88 754 27614.86 9.60 48.14 0.88- 0.80 754 42710.95 11.98 33.95 0.80- 0.75 754 21986.52 6.60 21.22 0.75- 0.71 754 19936.00 6.51 16.18 0.71- 0.67 754 26011.71 8.28 29.58 0.67- 0.62 754 3751.50 1.84 6.63 ------------------------------------------------------------------------------------ 6.00- 0.62 7540 46172.05 11.60 38.22 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\xs2212a\plots_red\xs2212a_absscale.dat Started at Wed Aug 21 15:26:20 2019 Sorting 7540 observations 43 unique observations with > 7.00 F2/sig(F2) 7540 observations in 8 runs Run # start # end # total # 1 0 102 103 2 0 102 206 3 0 101 308 4 0 103 412 5 0 103 516 6 1 98 614 7 0 46 661 8 0 98 760 Total number of frames 760 Maximum number of 43 frame scales suggested for reliable scaling Glued frame scales: 18 frame = 1 scale 7540 observations in 8 runs Run # start # end # total # 1 0 5 6 2 0 5 12 3 0 5 18 4 0 5 24 5 0 5 30 6 0 5 36 7 0 2 39 8 0 5 45 Total number of frames 45 1832 observations > 7.00 F2/sig(F2) 1832 observations in 8 runs Run # start # end # total # 1 0 5 6 2 0 5 12 3 0 5 18 4 0 5 24 5 0 5 30 6 0 5 36 7 0 2 39 8 0 5 45 Total number of frames 45 Removing 'redundancy=1' reflections Average redundancy: 31.0 (Out of 1832 removed 1 = 1831, unique = 59) 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 1831 observations in 8 runs Run # start # end # total # 1 0 5 6 2 0 5 12 3 0 5 18 4 0 5 24 5 0 5 30 6 0 5 36 7 0 2 39 8 0 5 45 Total number of frames 45 59 unique data precomputed (should be 59) 59 unique data with 1831 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 31.0 (Out of 1831 removed 0 = 1831, unique = 59) 59 unique data precomputed (should be 59) 59 unique data with 1831 observations RMS deviation of equivalent data = 0.31904 Rint = 0.25971 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.25290, wR= 0.34373 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13441, wR= 0.18277, Acormin=0.467, Acormax=1.455, Acor_av=0.976 F test: Probability=1.000, F= 3.530 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13440, wR= 0.17911, Acormin=0.453, Acormax=1.502, Acor_av=0.969 F test: Probability=0.000, F= 0.999 Trying model 3 (ne=4, no=0)... Results: Rint= 0.12510, wR= 0.17367, Acormin=0.556, Acormax=1.552, Acor_av=0.984 F test: Probability=0.998, F= 1.149 Trying model 4 (ne=4, no=1)... Results: Rint= 0.12534, wR= 0.16908, Acormin=0.519, Acormax=1.563, Acor_av=0.980 F test: Probability=0.000, F= 0.994 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10661, wR= 0.15009, Acormin=0.566, Acormax=1.829, Acor_av=1.011 F test: Probability=1.000, F= 1.369 Final absorption model (ne=4, no=3): Rint= 0.10661, Acormin=0.566, Acormax=1.829, Acor_av=1.011 Combined refinement in use Rint: 0.26156 There are 45 active scales (one needs to be fixed) Refinement control: frame scale #28 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 3 (24 parameters) Refinement control: 68 pars with 2346 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.31904 Using Levenberg-Marquardt: 0.00010 New wR= 0.10928 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25971 with corrections 0.08071 Rint for all data: 0.26156 with corrections 0.08342 4 observations identified as outliers and rejected Cycle 2 wR= 0.10055 Using Levenberg-Marquardt: 0.00001 New wR= 0.08480 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25977 with corrections 0.05954 Rint for all data: 0.26156 with corrections 0.06466 4 observations identified as outliers and rejected Cycle 3 wR= 0.07655 Using Levenberg-Marquardt: 0.00000 New wR= 0.07292 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25668 with corrections 0.05129 Rint for all data: 0.26156 with corrections 0.05773 1 observations identified as outliers and rejected Cycle 4 wR= 0.06989 Using Levenberg-Marquardt: 0.00000 New wR= 0.06856 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25626 with corrections 0.04900 Rint for all data: 0.26156 with corrections 0.05574 1 observations identified as outliers and rejected Cycle 5 wR= 0.06581 Using Levenberg-Marquardt: 0.00000 New wR= 0.06430 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.25607 with corrections 0.04739 Rint for all data: 0.26156 with corrections 0.05426 0 observations identified as outliers and rejected Final wR= 0.06430 Final frame scales: Min= 0.7160 Max= 1.3582 Final absorption correction factors: Amin= 0.3192 Amax= 1.6980 PROFFIT INFO: Inet (after scale3 abspack): min=-1209.8579 max=1296991.6250 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=41.4513 max=26359.4551 ****************************************************************************** * 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\xs2212a\xs2212a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/104 7540 reflections read from tmp file 279 reflections are rejected (278 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 1 1 2 1 1 2 3 151 Initial Chi^2= 0.51242 Cycle 1, Chi^2= 1.02239 Current error model SIG(F2)^2 = 61.78*I_RAW + 12.01*I_BACK+(0.02966*)^2 Cycle 2, Chi^2= 1.01013 Current error model SIG(F2)^2 = 73.10*I_RAW + 9.29*I_BACK+(0.02623*)^2 Cycle 3, Chi^2= 1.00294 Current error model SIG(F2)^2 = 76.17*I_RAW + 8.66*I_BACK+(0.02567*)^2 Cycle 4, Chi^2= 1.00070 Current error model SIG(F2)^2 = 76.90*I_RAW + 8.52*I_BACK+(0.02559*)^2 Cycle 5, Chi^2= 1.00016 Current error model SIG(F2)^2 = 77.07*I_RAW + 8.49*I_BACK+(0.02557*)^2 Final Chi^2= 1.00016 Final error model SIG(F2)^2 = 77.07*I_RAW + 8.49*I_BACK+(0.02557*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 1296992- 120400 754 388548.03 32.00 100.00 120096- 3552 754 30108.27 13.81 100.00 3551- 2068 754 2772.39 6.53 99.87 2067- 1195 754 1554.33 4.13 74.14 1195- 796 754 975.74 2.92 33.55 796- 537 754 662.76 2.48 17.64 537- 338 754 431.07 2.00 9.55 337- 158 754 249.60 1.47 4.38 158- 20 754 84.56 0.73 0.40 20- -1210 754 -139.62 -0.55 0.00 ------------------------------------------------------------------------------------ 1296992- -1210 7540 42524.71 6.55 43.95 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 754 104239.99 10.54 72.28 1.64- 1.26 754 82398.02 9.68 61.27 1.26- 1.06 754 72374.96 9.92 77.45 1.06- 0.96 754 37374.14 5.64 33.42 0.96- 0.88 754 25093.39 6.13 58.22 0.88- 0.80 754 39176.11 6.78 43.37 0.80- 0.75 754 19695.11 4.42 25.20 0.75- 0.71 754 18097.61 4.80 23.47 0.71- 0.67 754 23286.15 5.78 34.62 0.67- 0.62 754 3511.66 1.80 10.21 ------------------------------------------------------------------------------------ 6.00- 0.62 7540 42524.71 6.55 43.95 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6.00- 1.64 754 104239.99 10.54 72.28 6.00- 1.26 1508 93319.00 10.11 66.78 6.00- 1.06 2262 86337.65 10.05 70.34 6.00- 0.96 3016 74096.78 8.94 61.11 6.00- 0.88 3770 64296.10 8.38 60.53 6.00- 0.80 4524 60109.43 8.12 57.67 6.00- 0.75 5278 54335.96 7.59 53.03 6.00- 0.71 6032 49806.17 7.24 49.34 6.00- 0.67 6786 46859.50 7.08 47.70 6.00- 0.62 7540 42524.71 6.55 43.95 ------------------------------------------------------------------------------------ 6.00- 0.62 7540 42524.71 6.55 43.95 Scale applied to data: s=0.771014 (maximum obs:1296991.625,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.054; Rsigma 0.036: data 7540 -> merged 163 With outlier rejection... Rint 0.049; Rsigma 0.036: data 7522 -> merged 163 Rejected total: 18, method kkm 8, method Blessing 10 Completeness direct cell (a, b, c) = (10.408, 10.408, 10.408), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.621984, 6.008932 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 10.41 - 1.76 14 14 48.50 100.00 679 1.73 - 1.27 14 14 52.93 100.00 741 1.26 - 1.06 14 14 60.86 100.00 852 1.05 - 0.97 14 14 53.07 100.00 743 0.95 - 0.88 14 14 56.00 100.00 784 0.87 - 0.81 14 14 49.29 100.00 690 0.80 - 0.76 14 14 52.14 100.00 730 0.76 - 0.72 14 14 43.00 100.00 602 0.72 - 0.69 14 14 48.21 100.00 675 0.69 - 0.65 19 19 39.89 100.00 758 --------------------------------------------------------------- 10.41 - 0.65 145 145 50.03 100.00 7254 DELETE INFO: Deleting .hklgral file... (D:\Data\xs2212a\xs2212a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs2212a\xs2212a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Wed Aug 21 15:26:19 2019 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 10.406726 10.413986 10.402395 89.9944 90.0108 89.9792 7521 Reflections read from file xs2212a.hkl 7521 Reflections used for space-group determination (up to diffraction limit of 0.62A); mean (I/sigma) = 6.45 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 3772 0 4989 4989 7521 N (int>3sigma) = 0 0 0 0 1747 0 2278 2248 3256 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.5 31.8 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.6 6.5 6.5 Lattice type: F chosen Volume: 1127.36 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 0.5000 Unitcell: 7.356 7.358 7.359 119.99 119.96 90.02 Niggli form: a.a = 54.117 b.b = 54.138 c.c = 54.160 b.c = -27.065 a.c = -27.035 a.b = -0.023 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.097 CUBIC F-lattice R(int) = 0.050 [ 7280] Vol = 1127.4 Cell: 10.414 10.407 10.402 89.99 90.01 89.98 Volume: 1127.36 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.052 TETRAGONAL I-lattice R(int) = 0.050 [ 6882] Vol = 563.7 Cell: 7.360 7.363 10.402 90.00 89.99 89.96 Volume: 563.68 Matrix: 0.5000 -0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.039 TETRAGONAL I-lattice R(int) = 0.050 [ 6879] Vol = 563.7 Cell: 7.356 7.358 10.414 90.01 89.98 90.02 Volume: 563.68 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.049 TETRAGONAL I-lattice R(int) = 0.050 [ 6882] Vol = 563.7 Cell: 7.363 7.360 10.402 90.01 90.00 90.04 Volume: 563.68 Matrix:-0.5000 -0.5000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.041 ORTHORHOMBIC F-lattice R(int) = 0.049 [ 6828] Vol = 1127.4 Cell: 10.402 10.407 10.414 89.98 90.01 89.99 Volume: 1127.36 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.055 ORTHORHOMBIC I-lattice R(int) = 0.049 [ 6807] Vol = 563.7 Cell: 10.402 7.363 7.360 89.96 89.99 90.00 Volume: 563.68 Matrix: 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [42] err= 0.033 ORTHORHOMBIC I-lattice R(int) = 0.049 [ 6808] Vol = 563.7 Cell: 7.356 7.358 10.414 89.99 90.02 90.02 Volume: 563.68 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.023 MONOCLINIC I-lattice R(int) = 0.047 [ 6270] Vol = 563.7 Cell: 7.360 10.402 7.363 90.00 90.04 90.01 Volume: 563.68 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [14] err= 0.032 MONOCLINIC I-lattice R(int) = 0.048 [ 6269] Vol = 563.7 Cell: 7.359 10.407 7.360 90.01 90.06 89.98 Volume: 563.68 Matrix: 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.021 MONOCLINIC I-lattice R(int) = 0.047 [ 6270] Vol = 563.7 Cell: 7.363 10.402 7.360 90.01 90.04 90.00 Volume: 563.68 Matrix: 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [41] err= 0.023 MONOCLINIC I-lattice R(int) = 0.047 [ 6248] Vol = 563.7 Cell: 7.356 7.358 10.414 90.01 90.02 89.98 Volume: 563.68 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.014 MONOCLINIC I-lattice R(int) = 0.047 [ 6269] Vol = 563.7 Cell: 7.356 10.414 7.358 90.01 90.02 89.98 Volume: 563.68 Matrix: 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.025 MONOCLINIC I-lattice R(int) = 0.047 [ 6269] Vol = 563.7 Cell: 7.356 10.414 7.358 89.99 90.02 90.02 Volume: 563.68 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) = 0.044 [ 5195] Vol = 281.8 Cell: 7.356 7.358 7.359 119.99 119.96 90.02 Volume: 281.84 Matrix:-0.5000 0.0000 -0.5000 0.5000 0.0000 -0.5000 0.0000 -0.5000 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 3772 0 4989 4989 7521 N (int>3sigma) = 0 0 0 0 1747 0 2278 2248 3256 Mean intensity = 0.0 0.0 0.0 0.0 1.4 0.0 33.5 31.8 32.4 Mean int/sigma = 0.0 0.0 0.0 0.0 4.1 0.0 6.6 6.5 6.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 3.676 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 57 57 560 1473 N I>3s 2 2 3 803 0.0 0.0 -0.0 1.9 0.8 0.8 0.2 5.1 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 0.050 6748 Fd-3m 1 1 227 C N N N N 37 2284 0.050 6814 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=5.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs2212a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 10.413986 10.406726 10.402395 89.9892 90.0056 89.9792 ZERR 5.00 0.001186 0.001279 0.000906 0.0086 0.0083 0.0096 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 55.00 50.00 5.00 5.00 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\xs2212a\xs2212a.p4pgral! Back-up copy of original file: D:\Data\xs2212a\xs2212a.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 --------------------------------------------------------------------------------------------- 1160873- 96801 917 906 27 33.6 339584.70 30.24 0.046 0.058 78060- 1844 1410 1407 27 52.1 5395.44 8.77 0.080 0.095 1763- 798 1531 1529 27 56.6 1164.08 3.16 0.221 0.293 790- 362 1402 1401 27 51.9 523.49 2.11 0.357 0.509 336- 74 1143 1143 27 42.3 227.65 1.24 0.590 1.109 66- -206 1137 1136 28 40.6 8.60 0.17 0.959 4.197 ------------------------------------------------------------------------------------------- 1160873- -206 7540 7522 163 46.1 42281.09 6.53 0.049 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-1.27 1422 1418 27 52.5 98396.72 10.63 0.046 0.059 0.028 1.26-0.97 1600 1595 28 57.0 51248.47 7.36 0.043 0.055 0.033 0.95-0.81 1476 1474 28 52.6 32825.76 6.57 0.051 0.063 0.041 0.80-0.73 1306 1303 27 48.3 18628.85 4.53 0.057 0.071 0.052 0.72-0.67 1155 1153 27 42.7 18727.72 4.87 0.072 0.094 0.060 0.66-0.62 581 579 26 22.3 4350.48 1.93 0.105 0.085 0.117 ------------------------------------------------------------------------------------------------------ inf-0.62 7540 7522 163 46.1 42281.09 6.53 0.049 0.062 0.036 inf-0.65 7269 7252 144 50.4 43599.79 6.69 0.049 0.061 0.036 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-1.27 1418 27 27 100.0 52.5 98396.72 74.27 0.046 0.006 1.26-0.97 1595 28 28 100.0 57.0 51248.47 52.31 0.043 0.005 0.95-0.81 1474 28 28 100.0 52.6 32825.76 47.88 0.051 0.007 0.80-0.73 1303 27 27 100.0 48.3 18628.85 28.57 0.057 0.009 0.72-0.67 1153 27 27 100.0 42.7 18727.72 33.96 0.072 0.010 0.66-0.62 579 26 26 100.0 22.3 4350.48 9.07 0.105 0.025 -------------------------------------------------------------------------------------------- inf-0.62 7522 163 163 100.0 46.1 42281.09 45.33 0.049 0.007 inf-0.65 7252 144 144 100.0 50.4 43599.79 46.73 0.049 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs2212a\struct\olex2_xs2212a\.olex\originals\*.*) ? Olex report: D:\Data\xs2212a\struct\olex2_xs2212a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs2212a\struct\olex2_xs2212a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs2212a\struct\olex2_xs2212a\xs2212a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs2212a\xs2212a_proffitpeak"